TI: Analysis of toxic wastes in tissues from aquatic species. Applications of matrix solid-phase dispersion. AU: Crouch,-MD; Barker,-SA AD: Louisiana State Univ., Lab. Residue Studies, School Vet. Med., Baton Rouge, LA 70803, USA SO: J-Chromatogr,-A. 11 Jul 1997; 774(1-2): 287-309 AB: A review is presented that surveys problems of extraction of toxic waste components (such as PAH, PCB, organochlorine compounds and pesticides) from aquatic biological matrices (such as tissues from fish, shellfish and amphibians), including regulatory legislation. Toxic contaminants typically present in various biological species matrices are tabulated. The matrix solid-phase dispersion analysis of toxic agricultural compounds in four matrices and of PAH and PCB in one matrix (catfish muscle) is examined. Subsequent analyses of extracts are by GC or HPLC. Present developments in the field are described and future ones discussed. (175 references). Record 2 of 57
TI: Veterinary drug residues survey in meat: an HPLC method with a matrix solid-phase dispersion extraction. AU: Le-Boulaire,-S; Bauduret,-J-C; Andre,-F AD: Nestle France, Lab. Contole, 95806 Cergy Pontoise, France SO: J-Agric-Food-Chem. Jun 1997; 45(6): 2134-2142 AB: Meat was extracted using matrix solid-phase dispersion with C18. Two fractions were eluted with CH2Cl2 and ethyl acetate which were dried at 40degreeC. The respective residues were reconstituted with 0.01M-ammonium acetate buffer of pH 5.2/acetonitrile/methanol (43:5:2 and 56:31:13). HPLC was performed on a 5 micro m Spherisorb C18 ODS II column (25 cm x 4.6 mm i.d.) operated at 35degreeC with gradient elution (1 or 0.5 ml/min) with 0.01M-ammonium acetate buffer of pH 5.2/acetonitrile/methanol (details given for each fraction) and diode-array detection at 270 and 365 nm for the first fraction and 254, 291 and 348 nm for the second fraction. The second fraction was also detected by fluorescence at 365 nm (excitation at 308 nm). Calibration graphs were linear from 50-250 ppb and detection limits were The method was used to determine 14 veterinary drug residues in meat. Record 3 of 57
TI: Fluorodensitometric residue analysis of sulphaguanidine and sulphadimidine after MSPD-clean up of aluminium oxide. AU: Glaser,-B; Petz,-M AD: Bergische Univ. GH Wuppertal, Wuppertal, Germany SO: Lebensmittelchemie. 1996; 50(1): 9 AB: The use of C18 cartridges for the isolation of the sulphonamide drugs from animal samples gave poor recoveries because of irreversible adsorption. Subsequent HPLC determination also caused problems because of early elution, especially of sulphaguanidine. These problems were overcome by the use of the aluminium oxide matrix solid-phase dispersion (MSPD) technique of Barker etal. (J. Chromatogr., 1989, 475, 353). The sulphonamide drugs were eluted from the aluminium oxide with a mixture of acetonitrile and saturated Na2CO3 solution and were separated by TLC. The spots were located by dipping the plate in fluorescamine solution, with densitometric measurement of the fluorescence. This procedure gave 70-90% recovery of 50-200 ppb of the three sulphonamides from tissues and fluids without matrix interference. Record 4 of 57
TI: Optimization of matrix solid-phase dispersion method for the analysis of pesticide residues in vegetables. AU: Viana,-E; Molto,-JC; Font,-G AD: Univ. Valencia, Lab. Food Chem. and Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 437-444 AB: A multiresidue method based on matrix solid-phase dispersion was developed for extracting chlorfenvinfos, chlorpyrifos, fenarimol, iprodione, procimydone, propiconazole, tetradifon, triadimefon and vinclozolin from artichokes, green beans, lettuce and tomato. A mixture of 5 g chopped vegetables, 10 g Florisil (60-100 mesh) and 8 g acid washed sand was ground to a homogeneous flowing powder. The powder was transferred to an extraction column (40 cm x 3 cm i.d.) with 2 x 50 ml CH2Cl2. The CH2Cl2 extract was collected and reduced to 10 ml by evaporation at 60degreeC and the solvent was changed to 1 ml methanol. The extract was purified by SPE using octyl-silica Bondapak (37-55 micro m) and 5 ml ethyl acetate as eluent. The eluate was reduced to 1 ml and a 2 micro l portion was analysed by GC-ECD on a column (30 m x 0.25 mm i.d.) coated with DB-5 (0.25 micro m) with He as carrier gas (2.8 ml/min) and temperature programming from 50degreeC (held for 0.8 min) to 140degreeC (held for 2 min) at 30degreeC/min and then to 280degreeC (held for 12 min) at 5degreeC/min. The mean recovery of the target pesticides from vegetables spiked at the 18-95 ng/g level was 91% and the RSD were The method was used to analyse vegetables from local markets. Record 5 of 57
TI: Determination of pesticide residues in fruit and vegetables. AU: Torres,-CM; Pico,-Y; Manes,-J AD: Univ. Valencia, Lab. Bromatol. i Toxicol., Fac. Farm., 46100 Burjassot, Valencia, Spain SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 301-331 AB: A review is presented on methods based on GC, HPLC, SFC and immunoassay for determining pesticide residues in fruit and vegetables. Extraction and clean up procedures by liquid-liquid extraction, matrix solid-phase dispersion and SFE are discussed. (185 references). Record 6 of 57
TI: Pesticide residue analyses in plant material by chromatographic methods: clean up procedures and selective detectors. AU: Tekel,-J; Hatrik,-S AD: Comenius Univ., Fac. Pharm., 832 32 Bratislava, Slovakia SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 397-410 AB: A review is presented of GC and LC methods for determining pesticide residues in plant materials. Extraction and clean up procedures based on adsorption column chromatography, GPC, SFE, matrix solid-phase dispersion and sweep co-distillation are discussed. (99 references). Record 7 of 57
TI: Determination of polychlorinated biphenyls and chlorinated pesticides in human body fluids and tissues. AU: Bucholski,-KA; Begerow,-J; Winneke,-G; Dunemann,-L AD: Med. Inst. Umwelthygiene, Dept. Anal. Chem., 40225 Duesseldorf, Germany SO: J-Chromatogr,-A. 22 Nov 1996; 754(1-2): 479-485 AB: A single-stage clean up preconcentration procedure based on matrix solid-phase dispersion was employed in determining PCB and chlorinated pesticides in human blood serum, milk, bone marrow and tissue. Samples of up to 5 ml or 1 g were homogenized with up to 6 g activated Florisil (0.15-0.25 mm particle size). The resulting powder was transferred to a prepacked column (2.2 cm i.d.) containing up to 15 g Florisil deactivated with 3% H2O. The column was washed with 60 ml hexane and 80 ml hexane/CH2Cl2 (4:1). Both eluates were collected, combined and reduced to 0.5 ml for analysis by GC-MS or dual-column GC with ECD. Analysis by GC-MS was performed on
a column (50 m x 0.2 mm i.d.) coated with Ultra 2 (0.33 micro m) coupled directly to a quadrupole MS operated in the selected-ion monitoring mode. The dual-column GC was equipped with a column (30 m x 0.32 mm i.d.) coated with DB5-MS (0.25 micro m) and a column (30 m x 0.32 mm i.d.) coated with DB-1701 (0.25 micro m) operating in parallel and two 63Ni electron-capture detectors. The detection limits for chlorinated pesticides and PCB congeners were 1.3-4 pg and 1- 23.3 pg, respectively, for GC-MS and 0.4-0.8 pg and 0.3-0.7 pg, respectively, for dual-column GC. Record 8 of 57
TI: Matrix solid-phase dispersion technique for the determination of moxidectin in bovine tissues. AU: Alvinerie,-M; Sutra,-JF; Capela,-D; Galtier,-P; Fernandez-Suarez,-A; Horne,-E; O'Keeffe,-M AD: INRA, Lab. Pharmacol.-Toxicol., 31931 Toulouse, France SO: Analyst (Cambridge, UK). Oct 1996; 121(10): 1469-1472 AB: Homogenized bovine tissue (muscle, liver) (0.25 g) was blended with 1 g C18 end-capped sorbent. A column was prepared with the resulting material and was washed with 2 ml hexane. After drying the column, moxidectin (I) was eluted with 6 ml CH2Cl2/ethyl acetate (3:1) onto an Alumina-B SPE cartridge attached below the column. The SPE cartridge was dried, washed with 1 ml acetone and dried again, after which I was eluted with 6 ml methanol. The eluate was evaporated to dryness and the residue was treated with N-methylimidazole and trifluoroacetic anhydride in acetonitrile (cf. Alvinerie et al., J. Chromatogr. B., 1995, 674, 119). A portion (100 micro l) of the reaction mixture was analysed by HPLC on a 3 micro m Supelcosil column (15 cm x 4.6 mm i.d.), with 0.2% acetic acid/methanol/acetontrile (4:15:31) as mobile phase (1.5 ml/min) and fluorimetric detection at 447 nm (excitation at 383 nm). The calibration graph was linear for 1 (detection limit) to 100 ng/g of I. The inter-assay RSD (n = 5) was Recoveries of I were >80%. Record 9 of 57
TI: Preparation of sample solution for determination of acid coal-tar dyes in confectionery by the matrix solid-phase dispersion method. AU: Kai,-S; Nikkawa,-T; Takahashi,-A; Koizumi,-A; Hyoudou,-Y; Suzuki,-S; Nakazawa,-H AD: Kanagawa Prefectural Chigasaki Health Centre, Kanagawa 253, Japan SO: Shokuhin-Eiseigaku-Zasshi. Jun 1996; 37(3): 146-150 AB: Sample (0.5 g) was treated with 0.7 ml methanolic 0.1M-cetyltrimethylammonium bromide (I) and blended with 2 g octadecylsilyl (C18)-derivatized silica (50 micro m; C18-Sil) as adsorbent and dried. The C18-Sil and prepared sample matrix were respectively packed into a small column for percolation with 10 ml H2O. The food dyes (food colourings; FC) were eluted with 5 ml methanol through a syringe. For qualitative analysis, the eluate was directly applied on to a Kiesel Gel 60 plate for TLC with ethyl acetate/methanol/28% ammonia H2O (3:3:1) as mobile phase. For quantitative analysis, the eluate was diluted 5-fold with mobile phase, centrifuged for 5 min and a 20 micro l portion of the supernatant was analysed by HPLC on a Finepak C-18S column (15 cm x 4.6 mm i.d.) operated at 50degreeC with aqueous 77% methanol, containing 25 mg/ml I, as mobile phase (1 ml/min) and detection at 254 nm. The method was used for the determination of 12 permitted and 4 non-permitted FC (tabulated) in soft-drink powder, candy, chewing gum and cookie. By standard-additions method, recoveries were 76.7-102.4%. Record 10 of 57
TI: Latest analytical methods for the residual pesticides in food. AU: Obana,-H; Hori,-S AD: Osaka Prefectural Inst. Public Health, Osaka 537, Japan SO: Jpn-J-Toxicol-Environ-Health. Feb 1996; 42(1): 1-16 AB: A review is presented of the analysis of pesticides in food at sub-ppm levels. Extraction techniques of matrix solid phase dispersion and SFE, clean up procedures of miniature size column and gel permeation chromatography and analysis by GC and GC-MS are described. The importance of multiresidue analysis is commented on. (52 references). Record 11 of 57 ;
TI: Matrix solid-phase dispersion extraction procedure for multiresidue pesticide analysis in oranges. AU: Torres,-CM; Pico,-Y; Redondo,-MJ; Manes,-J AD: Valencia Univ., Lab. Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain SO: J-Chromatogr,-A. 5 Jan 1996; 719(1): 95-103 AB: The optimization of a matrix solid-phase dispersion method for detection of 18 insecticides in oranges was studied, with subsequent determination by GC. Milled whole orange and C18 silica (each 0.5 g) plus 0.5 ml insecticide in ethyl acetate (when testing method efficiency) were homogenized and transferred on to silica (0.5 g) in a glass column (10 cm x 9 mm i.d.) and the pesticide was eluted with 10 ml ethyl acetate for analysis by GC in a column (30 m x 0.25 mm i.d.) coated with DB-1 (0.25 micro m) operated with temperature programming from 50degreeC (held 0.8 min) by multistep gradient (details given) to 280degreeC (held for 1 min), with He as carrier gas (1 ml/min) and ECD. The lower limits of detection ranged from 2 ppb for aldrin to 171 ppb for captafol. Test recoveries ranged from 48+/-5% for tetradifon to 108+/-5% for chlorpyriphos. Test recovery for each pesticide is tabulated alongside recoveries obtained by three established liquid- liquid extraction methods. Record 12 of 57
TI: Methods for the determination of beta-agonists in biological matrices. AU: Boyd,-D; O'Keefe,-M; Smyth,-MR AD: Natl. Food Centre, Dublin 15, Ireland SO: Analyst (Cambridge, UK). Jan 1996; 121(1): 1R-10R AB: A review is presented of methods for determining beta-agonists in complex biological samples. Emphasis is placed on sample purification procedures, e.g., solvent extraction and liquid-liquid partitioning, SPE, immunoaffinity chromatography and matrix solid-phase dispersion. Detection techniques for beta-agonists, e.g., HPLC, GC-MS and immunoassays, are also discussed. (115 references). Record 13 of 57 ;
TI: Analysis of pesticide residues in fruit and vegetables by matrix solid-phase dispersion (MSPD) and different gas chromatography element-selective detectors. AU: Torres,-CM; Pico,-Y; Manes,-J AD: Valencia Univ., Lab. Bromatol. Toxicol., Fac. Pharm., 46100 Burjassot, Valencia, Spain SO: Chromatographia. Dec 1995; 41(11-12): 685-692 AB: Samples (0.5 g) were chopped and mixed before blending with C18 silica. The homogenate was applied to a glass column (10 cm x 9 mm i.d.) packed with 1.5 g silica. Ethyl acetate (10 ml) was added and the effluent (15 ml) was collected and concentrated under N2 to 0.5 ml. Portions (1-2 micro l) of the extract were analysed by GC with a number of different detection methods viz., ECD, N-P detection, flame-photometric detection, (S and P modes) and mass-selective detection in selected-ion monitoring mode. Three GC systems were used: (i) a DB-5 column (30 m x 0.25 mm i.d.; 0.25 micro m) equipped with an ECD and flame-photometric detector; (ii) a DB-1 column (30 m x 0.25 mm i.d.) equipped with an ECD and a N-P detector; (iv) a BPX-5 column (25 m x 0.22 mm i.d. 0.25 micro m) equipped with a mass spectrometer. Analysis was performed with temperature programming from 50degreeC (held for 0.8 min) to 100degreeC (held for 2 min) with 30degreeC/min, then to 180degreeC at 10degreeC/min, and then to 280degreeC (held for 5 min) at 4degreeC/min. The use of the detectors in parallel was also investigated. Recoveries were 41- 108% with RSD of 2-14% over the concentration range 0.5-10 micro g/l. Record 14 of 57 ;
TI: Screening procedure for organochlorine and organophosphorus pesticide residues in milk using matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic determination. AU: Schenck,-FJ; Wagner,-R AD: Food and Drug Administration, Baltimore, MD 21201, USA SO: Food-Addit-Contam. Jul-Aug 1995; 12(4): 535-541 AB: Milk (5 ml) was blended with 2 g preconditioned C18 silica and 1.5 ml acetonitrile in a syringe barrel. The aqueous phase was removed from the column by vacuum aspiration and the pesticides were eluted with 20 ml acetonitrile directly onto a Florisil SPE column (2 g) containing a top 3 cm layer of Na2SO4. The eluates were evaporated to dryness under N2 and the residue was dissolved in 1 ml petroleum ether (solution A). Portions (3 micro l) were analysed by GC for organochlorine (OC) pesticides (tabulated) on a capillary column (30 m x 0.53 mm i.d.) coated with DB-608 (1.5 micro m) operated at 190degreeC with He as carrier gas (20 ml/min) and 63Ni ECD. Portions (3 micro l) of solution A were also analysed for organophosphorus (OP) pesticides on a capillary column (30 m x 0.53 mm i.d.) coated with DB-1 (1.5 micro m) operated at 185degreeC with He as carrier gas (10 ml/min) and flame-photometric detection. Recoveries were 76-97.8 and 75-104.5%, respectively, for milk spiked with 2-20 and 10-50 ppb, respectively of OC and OP pesticides. Results for OC pesticides agreed well with those obtained by the AOAC International multiresidue method of Sawyer et al. (Official Methods of Analysis of the Association of Official Analytical Chemists, 1990, 15th edition, Helrich, K. (ed.), 274). Record 15 of 57 ;
TI: Matrix solid-phase dispersion linked to solid-phase extraction for beta-agonists in liver samples: an update. AU: Boyd,-D; O'Keeffe,-M; Smyth,-MR AD: Natl. Food Centre, Dublin 15, Ireland SO: Anal-Proc. Aug 1995; 32(8): 301-303 AB: Liver (500 mg) was dissolved in 10 micro l ethanol and the solution was spiked with 2 ng each of salbutamol (I), clenbuterol (II) and mabuterol (III). The solution was blended with 50 micro m Isolute C18 and 40 micro m Bondesil C18 solid phases and packed into columns. I, II and III were eluted with 12 ml methanol. The eluates were centrifuged at 2000 rpm for 10 mins and the supernatants were evaporated to dryness at 60degreeC under N2. The residues were dissolved in 400 micro l phosphate-gelatin buffer of pH 5, 100 micro l Helix pomatia solution (1:9) was added and the extracts were incubated at 37degreeC for 2h. On cooling, 500 micro l H2O and 80 micro l 1M-NaOH were added to the incubates and the solutions were applied to a C18 SPE cartridge. The drugs were eluted with 2 ml methanol, the eluates were evaporated under N2 at 60degreeC and the residues were dissolved in 500 micro l phosphate-gelatin buffer of pH 7. Portions (0.1 ml) were analysed by RIA by the method of Boyd et al. (Analyst (Cambridge, UK), 1994, 119, 1467). Mean recoveries were 79-90, 93-135 and 81-81%, respectively, for I, II and III at 1-2 ng of added drug. The corresponding RSD (n = 5) were 11.7-26.2, 19.1-25.7 and 8.7-15.9%. Detection limits were 0.17 and 0.57 ng/g, respectively of each drug on the Bondesil and Isolute C18 columns. Record 16 of 57
TI: Multiresidue matrix solid-phase dispersion method for the determination of six synthetic pyrethroids in vegetables followed by gas chromatography with electron-capture detection. AU: Ling,-Y-C; Huang,-I-P AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu 30043, Taiwan SO: J-Chromatogr,-A. 24 Mar 1995; 695(1): 75-82 AB: A 5 g portion of chopped vegetable was ground with 8 g of Florisil and applied to a glass column (30 cm x 15 mm i.d.) of anhydrous Na2SO4 (1 cm) and 0.5 g of Florisil compressed to a bed depth of 13 cm then covered with Na2SO4 (0.1-0.2 cm). Elution was with 60 ml of acetone/hexane (1:9). The eluate was concentrated to 2, 100 micro l of tribromobiphenyl was added (internal standard 3.9 micro g/ml) and the solution was diluted to 1 ml and analysed on a 0.25 micro m DB-5 MS column (30 m x 0.25 mm i.d.) with He as carrier gas at 1 ml/min and with
temperature programming from 60-220degreeC at 30degreeC/min and from 220-300degreeC at 3degreeC/min with detection by 70 eV EIMS using a Shimadzu QP-1000 EX MS system. The method was suitable for the simultaneous determination of fenpropathrin, cyhalothrin, permethrin, cypermethrin, fenvalerate and deltamethrin. Recoveries were 92-113% and detection limits were 5.1-91.5 ng/g for the cited insecticides in vegetables. The method is proposed as a relatively rapid screening technique for pyrethroids in vegetables. Record 17 of 57
TI: Isolation and quantification of ivermectin in bovine milk by matrix solid phase dispersion (MSPD) extraction and liquid-chromatographic determination. AU: Schenck,-FJ AD: US Food and Drug Administration, Baltimore District Lab., Baltimore, MD 21201, USA SO: J-Liq-Chromatogr. Jan 1995; 18(2): 349-362 AB: Milk (25 ml) was fortified with 50-400 micro l ng/ml ivermectin (500 ng/ml; I) solution and 200 micro l of 500 ng/ml abamectin solution (internal standard) was added. A 5 ml portion of the solution was blended with 2 g C18 Bondesil (40 micro m) for 2 min. The aqueous phase was removed and I was eluted with 10 ml ethyl acetate. The eluate was evaporated to dryness at 2. The residue was reconstituted in 2 ml 40% ethyl acetate in hexane and the solution was cleaned up on a Bond-Elut SPE column (500 mg). I residues were eluted from the SPE column with 5 ml of 50% ethyl acetate in methanol. The eluate was evaporated to dryness at The residue was derivatized with 0.1 ml DMF/acetic anhydride/N-methylimidazole (9:3:2) at 95degreeC for 1 h. The reaction mixture was diluted with 1 ml CHCl3, loaded on to a SPE column and the I residues were eluted with 2 ml CHCl3. The eluate was evaporated to dryness at A 50 micro l portion was injected on to a 5 micro m Econosil C18 (25 cm x 4.6 mm i.d.) column was used with a Brownlee Newguard RP-18 guard column, with methanol/THF/H2O (17:3:1) as mobile phase (1 ml/min), and fluorescence detection at 455 nm (excitation at 364 nm). Recoveries of 1-8 ppb I from milk were 81-91.5% and the RSD (n = 7) were 4.6-10.3%. Record 18 of 57
TI: Multiresidue-matrix solid-phase dispersion method for determining 16 organochlorine pesticides and polychlorinated biphenyls in fish. AU: Ling,-Y-C; Huang,-I-P AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu, 30043, Taiwan SO: Chromatographia. Mar 1995; 40(5-6): 259-266 AB: Fish fillet (0.5 g) was blended with 2 g C18 and the resulting material was placed in a glass syringe barrel containing 1 g Florisil at the bottom. Elution was effected under gravitational flow with n-hexane/acetone (9:1) and after the flow ceased the excess eluent was removed from the column under vacuum. The eluate was concentrated to 2 and 50 micro l dibromo- octafluorobiphenyl solution in n-hexane (4 ppm; internal standard) was added and the volume was adjusted to 100 micro l. The eluate was analysed by GC on a column (30 m x 0.25 mm i.d.) coated with DB-SMS (0.25 micro m) operated with temperature programming from 70degreeC (held for 2 min) to 180degreeC (held for 2 min) at 20degreeC/min, and then to 300degreeC (held for 4 min) at 10degreeC/min, with He as carrier gas (1 ml/min) and 70 eV EIMS detection (m/z tabulated). Detection limits were 19.6-91.1 ng/g and 71.4-111.2 ng/g for organochlorine pesticides and PCB, respectively. Recoveries were >85% for all the organochlorine pesticides except heptachlor (78%) and 4,4'-DDT (81%); recoveries of >95% were obtained for PCB. Record 19 of 57
TI: Matrix solid-phase dispersion and high-performance liquid-chromatographic determination of trace isoprocarb and deltamethrin. AU: Yang,-R; Fu,-CG AD: Hebei Univ., Res. Centre Phys. and Chem. Anal., Baoding 071002, China SO: Sepu. Nov 1994; 12(6): 431-432, 435 AB: Food sample (0.5 g) was ground with ODS bonded phase (100-140 mesh) and packed into a glass syringe. The column was washed with 8 ml cyclohexane, deltamethrin (I) and isoprocarb (II) were eluted with 6 ml toluene. The eluate was evaporated to dryness, the residue was dissolved in 500 micro l methanol and the solution was centrifuged at 1700 rpm for 10 min. Portions (10 micro l) of the supernatant were analysed by HPLC on a 5 micro m PE HS-5 C18 column (12.5 cm x 4.6 mm i.d.) with aqueous 65% methanol as mobile phase (1 ml/min) and detection at 254 nm. Calibration graphs were linear from 19-508 and 30-900 ng, for I and II, respectively. Average recoveries (n = 5) were 88.11+/-4.78 and 81.92+/-4.11%, respectively, for I and II. The method was applied to the determination of I and II in fruits and cereals. Record 20 of 57
TI: Novel approach to the "on-site" testing for sulfamethazine in pork carcasses. AU: Shearan,-P; O'Keeffe,-M AD: Natl. Food Centre, Dublin 15, Ireland SO: Analyst (London). Dec 1994; 119(12): 2761-2764 AB: Porcine muscle was extracted by matrix solid phase dispersion (MSPD), as described by Shearan et al. (FoodAddit. Contam., 1994, 11, 7). Elution of the analyte from the MSPD column was effected with 8 ml CH2Cl2. Petroleum spirit (3 ml) was added to the eluate, which was then loaded on to a 10 mg silica microcolumn, previously conditioned with 500 micro l of petroleum spirit; elution was effected with 150 micro l methanol. A portion (40 micro l) of the eluate was analysed by TLC on plates (10 x 10 cm) coated with silica gel 60, with a mobile phase of methanol for the first run and ethyl acetate for the second run, and detection at 366 nm after spraying with fluorescamine solution. The quantification limit was 30 ppb of sulfamethazine (sulphadimidine). The method was used for the "on-site" detection of sulfamethazone residues in pork carcasses at or below the maximum residue limit of 100 ppb. Record 21 of 57
TI: Automated extraction of acetylgestagens from kidney fat by matrix solid-phase dispersion. AU: Rosen,-J; Hellenas,-K-E; Tornqvist,-P; Shearan,-P AD: Natl. Food Administration, 751 26 Uppsala, Sweden SO: Analyst (London). Dec 1994; 119(12): 2635-2637 AB: Bovine kidney fat (0.5 g) was mixed with [3H]medroxyprogesterone acetate (internal standard) ground to a thin film, blended with 2 g of Bondesil C18 (40 micro m; Varian) and packed into an SPE column. The resulting matrix solid-phase dispersion (MSPD) column was loaded into a Gilson ASPEC unit for automated washing and elution. A Bond-Elut C18 SPE column was also loaded for further clean-up. The MSPD column was washed with 12 ml cyclohexane, dried with N2 and gestagens were eluted with 8 ml aqueous 80% methanol. The eluate was diluted with H2O to obtain a 50% methanol solution and applied to the activated Bond Elut column, which was washed with 9.5 ml aqueous 50% methanol before elution was effected with 3.5 ml aqueous 80% methanol. After evaporation, the extract was dissolved in 200 micro l aqueous 20% methanol for liquid scintillation counting. Alternatively, portions (20 micro l) were screened using an EIA kit (Ridascreen, Darmstadt, Germany). The recoveries of medroxyprogesterone acetate were 59% +/- 5%; similar results were obtained for chlormadinone acetate and megestrol acetate. The EIA detection limits were 1-2 ng/g. Record 22 of 57 ;
TI: Application of the matrix solid-phase dispersion technique for the determination of ivermectin residues in fish muscle tissue. AU: Iosifidou,-E; Shearan,-P; O'Keeffe,-M AD: Aristotle Univ., Dept. Food Hygiene and Technol., School Vet. Med., 540 06 Thessaloniki, Greece SO: Analyst (London). Oct 1994; 119(10): 2227-2229 AB: Homogenized tissue (0.5 g) was blended with 2 g C18 end-capped packing material for 45 s. The mixture was packed into a 10 ml syringe barrel and the resulting column was washed with 8 ml hexane. Ivermectin (I) was eluted with 8 ml CH2Cl2/ethyl acetate (3:1) and the eluate was evaporated to dryness under N2. The residue was dissolved in 1 ml methanol and the solution was filtered. A 500 micro l portion of the filtrate was evaporated to dryness and 100 micro l 1- methylimidazole/acetic anhydride/DMF (2:6:9) was added. The mixture was heated at 95degreeC for 1 h, cooled and 1 ml CHCl3 was added. The solution was applied to a Sep-Pak silica cartridge and the eluate collected. The column was washed with 9 ml CHCl3 and the eluate collected. The combined eluates were evaporated to dryness and the residue was dissolved in 250 micro l methanol. The solution was filtered and a 100 micro l portion of the filtrate was analysed by HPLC on a Novapak C18 column (15 cm x 3.9 mm i.d.) with a micro Bondpak C18 guard column with 97% aqueous methanol as mobile phase (1 ml/min) and fluorescence detection (excitation and emission wavelengths not given). The calibration graph was linear from 5-200 ng/ml of I. Intra- and inter-assay RSD (n = 3 or 4) were 6.9-7.8 and 5.5-13.1%, respectively. Recoveries were >80%. Record 23 of 57
TI: High-performance liquid-chromatographic analysis of sulfonamides in livestock products using matrix solid-phase dispersion (MSPD) method with silica gel. AU: Tamura,-H; Yotoriyama,-M; Kurosaki,-K; Shinohara,-N AD: Tochigi Prefectural Inst. Public Health, Food Div., Tochigi 320, Japan SO: Shokuhin-Eiseigaku-Zasshi. Jun 1994; 35(3): 271-275 AB: Sample (0.5 g) was mixed with 0.7 g silica gel and 0.5 g Na2SO4 in 1.5 ml acetonitrile then dried and applied to a Bond Elut reservoir containing a bed of Na2SO4 with hexane for washing and methanol or THF for elution (for analysis of meat or egg). The eluate was centrifuged at 4000 rpm for 2 min; the supernatant solution was evaporated to dryness. The residue was dissolved in 200 micro l methanol and then 10 micro l of the filtered solution was analysed by HPLC on a column (15 cm x 4.6 mm i.d.) operated at 40degreeC with acetonitrile/1% acetic acid (9:41) as mobile phase (1 ml/min) and detection at 272 nm. Detection limits for sulfameradine, sulfadimidine, sulfamonomethoxine, sulfadimethoxine and sulfaquinoxarine were 0.01-0.04 ppm. Recoveries were 69.6%-93.1%. The method was employed in assay of pork, chicken meat and egg. Record 24 of 57
TI: Extraction and liquid chromatographic analysis of sulfadimethoxine and 4-N- acetylsulfadimethoxine residues in channel catfish (Ictalurus punctatus) muscle and plasma. AU: Walker,-CC; Barker,-SA AD: Louisiana State Univ., Lab. Residue Studies, Dept. Vet. Physiol., Pharm. and Toxicol., School Vet. Med., Baton Rouge, LA 70803-8420, USA SO: J-AOAC-Int. Nov-Dec 1994; 77(6): 1460-1466 AB: Muscle was extracted using matrix solid-phase dispersion (MSPD) and plasma with a modified MSPD method in which 100 micro l plasma was vortex-mixed with 400 mg C18 in a disposable chromatographic column. Analysis was by LC on a 5 micro m ODS Hypersil column (20 cm x 2.1 mm i.d.) with 0.017M-aqueous H3PO4 of pH 2.4/acetonitrile as mobile phase (71:29 for muscle analysis and 73:27 for plasma analysis) as mobile phase (0.4 ml/min) and photodiode-array detection set at 265 nm with a reference spectrum of 45 nm and a spectrum range of 210-320 nm. A 10 micro l portion of muscle extract and a 25 micro l portion of plasma extract was used. Recoveries were 79 and 67% for muscle and plasma, respectively. Detection limits were 26 ng
sulphadimethoxine and 26 ng acetyl sulphadimethoxine/g muscle and corresponding plasma values were 33 and 11 ng/ml. Intra- and inter-assay RSD were Record 25 of 57
TI: Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion. AU: Barker,-SA; Long,-AR AD: Louisiana State Univ., Dept. Physiol., Pharmacol. and Toxicol., Baton Rouge, LA 70803-8420, USA SO: J-AOAC-Int. Jul-Aug 1994; 77(4): 848-854 AB: Sample (0.5 g) was blended with C18, internal standards or sample modifying agents (e.g., acids, bases, or chelators) for ~30 s. The semi-dry blend was applied to a 10 ml syringe barrel containing a paper frit. The column head was covered with a filter paper disc and the contents were compressed with a plunger to 4.5 ml. A disposable pipette tip on the end of the column increased the residence time of eluting solvents on the column. Elution was effected with 9 ml of a given solvent and 3-9 ml each of a series of solvents. The method can be used to increase the specificity of drug immunoassays by fractionating any drugs that may cross-react. Specific drug extraction and analysis procedures for several drugs used in dairy production are given. The method can also be used for LC screening and confirmation of a suspect sample. Record 26 of 57
TI: Solid phase techniques in the extraction of pesticides and related compounds from foods and soils. AU: Pico,-Y; Molto,-JC; Manes,-J; Font,-G AD: Univ. Valencia, Lab. Toxicol., Fac. Farm., 46100 Burjassot, Valencia, Spain SO: J-Microcolumn-Sep. Jul-Aug 1994; 6(4): 331-359 AB: A review is presented of the extraction of pesticides from milk, meat, sea-food, animal fat, vegetable oils, lanolin, fruits, vegetables and soil. The techniques of solid-phase extraction, solid- phase clean up and matrix solid phase dispersion are described. Tables are presented of the extraction and clean up procedures and the pesticide extracted for 64 matrices with recoveries, concentration ranges, detection limits, detectors used and references given. (97 references). Record 27 of 57
TI: Matrix solid-phase dispersion as a multiresidue extraction technique for beta-agonists in bovine liver tissue. AU: Boyd,-D; O'Keeffe,-M*; Smythe,-R AD: Natl. Food Centre, Dublin 15, Ireland SO: Analyst (London). Jul 1994; 119(7): 1467-1470 AB: Salbutamol residues in bovine liver were determined at sub ppb level by combining matrix sold-phase dispersion with RIA. Extraction was performed on a Sepralyte C18 column. A RIA kit with antiserum raised against salbutamol and an EIA kit with antiserum raised against clenbuterol were used. The scintillation cocktail was Cocktail T. Good recoveries of salbutamol were obtained from 1-5 ppb. An enzyme hydrolysis procedure was optimized for deconjugating the residue incurred. The method described was suitable for extracting and determining other beta-agonists (sympathomimetics) such as clenbuterol, mabuterol, terbutaline and cimaterol at levels of Record 28 of 57 ;
TI: Matrix solid-phase dispersion extraction and gas-chromatographic screening of polychlorinated biphenyls in fish. AU: Ling,-Y-C; Chang,-M-Y; Huang,-I-P AD: Natl. Tsing Hua Univ., Dept. Chem., Hsinchu 30043, Taiwan SO: J-Chromatogr-A. 27 May 1994; 669(1-2): 119-124 AB: Fillet of grass carp (0.5 g) was homogenized with 2 g of ODS silica (40 micro m), the mixture was packed into a 5 ml column and analytes were eluted with hexane (10 ml). The eluate was concentrated to 1 ml and a portion of the concentrate was injected on to a column (30 m x 0.53 mm i.d.) coated with DB-1 (1 micro m), operated with temp. programming from 170degreeC (held 3 min) to 300degreeC at 5degreeC/min with Ar/CH4 (19:1) as carrier gas (8 ml/min) and 63Ni ECD. Alternatively analysis was performed by GC-MS on a column (30 m x 0.25 mm i.d.) coated with DB-5 (0.25 micro m), operated with temp. programming from 70degreeC (held 5 min) to 180degreeC (held for 3 min) at 20degreeC/min, and then at 10degreeC/min to 320degreeC (held 6 min) and 70-eV EIMS. Test recoveries of various PCB at 0.6 ppm were evaluated. Mean recoveries (n = 4) of main components were 89.1+/-2.0% for trichloro-PCB and 93.2+/-4.3% for tetrachloro-PCB from KC-300 and 92.8 +/- 3.5% for pentachloro-PCB and 84.9 +/- 5.8% for hexaclore-PCB from KC-500. Results are discussed. Record 29 of 57 ;
TI: Comparison of matrix solid phase dispersion (MSPD) with a standard solvent extraction method for sulphamethazine in pork muscle using high-performance liquid and thin-layer chromatography. AU: Shearan,-P; O'Keeffe,-M; Smyth,-MR AD: Natl. Food Centre, Dublin 15, Ireland SO: Food-Addit-Contam. Jan-Feb 1994; 11(1): 7-15 AB: In the cited MSPD extraction/clean up procedure, pork tissue, unfortified or fortified with sulphamethazine (I; sulphadimidine) at 0.05 and 0.1 micro g/g, was blended with C18 resin in a mortar for 30-45 s. The blend was then packed into a syringe barrel, washed with hexane and elution was effected with CH2Cl2. The purified extract was analysed (i) by HPLC on a stainless- steel column (30 cm x 3.9 mm i.d.) of micro Bondapak C18 with a similar guard column, a mobile phase (no flow rate given) of acetonitrile/10mM-ammonium acetate of pH 6.8 (1:3) and detection at 254 nm; and (ii) after solvent evaporation and reconstitution in methanol or after back extraction with 0.01M-NaOH, by TLC on plates of silica gel 60 utilizing a modification of the Sulpha-on-Site test system with detection by spraying with fluorescamine in acetone followed by visualization at 366 nm. The extracts were free from interferences and the recovery of I was >80%. Using HPLC the calibration graph was linear for 0.025-1 micro g/ml of I and the detection limit was 0.025 micro g/g. Residue levels found compared well with those obtained using a conventional extraction/silica and C18 clean up method. Record 30 of 57
TI: Matrix solid-phase dispersion extraction and the analysis of drugs and environmental pollutants in aquatic species. AU: Walker,-CC; Lott,-HM; Barker,-SA AD: Louisiana State Univ., Lab. Residue Studies, School Veterinary Med., Baton Rouge, LA 70803, USA SO: J-Chromatogr. 16 Jul 1993; 642(1-2): 225-242 AB: A review is presented of methods for the extraction and determination of drugs and chlorinated pesticide residues in tissues of aquatic resources. Problems ocurring in the sample prep., isolation and cleanup stages are discussed and future methods of residue analysis, viz., solid-phase extraction, SFE and matrix solid-phase dispersion are described. (138 references). Record 31 of 57
TI: Liquid-chromatographic analysis of antibacterial drug residues in food products of animal origin. AU: Shaikh,-B; Moats,-WA AD: Center Veterinary Med., Food and Drug Administration, Beltsville, MD 20705, USA SO: J-Chromatogr. 23 Jul 1993; 643(1-2): 369-378 AB: A review is presented of recent developments in the LC determinations of antibiotic residues (e.g., aminoglycosides, chloramphenicol, sulfonamides, tetracyclines, macrolides, beta-lactams etc.) in food products of animal origin, e.g., meat or milk. Topics covered include cleanup procedures such as ultrafiltration, liquid-liquid parition, solid-phase extraction, immunoaffinity and matrix solid-phase dispersion as extraction, deproteination and concn. steps. (97 references). Record 32 of 57
TI: Determination of sulphamethazine in animal tissues by enzyme immunoassay. AU: Renson,-C; Degand,-G; Maghuin-Rogisster,-G; Delahaut,-P AD: Univ. Liege, Lab. Anal. Denrees Aliment. Origin Animale, Fac. Med. Vet., 4000 Liege, Belgium SO: Anal-Chim-Acta. 1 Apr 1993; 275(1-2): 323-328 AB: Muscle and liver from animals used for human consumption were prepared by matrix solid- phase dispersion as previously described (Long Austin et al., J. Agric. Food Chem., 1990, 38, 423). Extracts or standard soln. (50 micro l) and sulphamethazine (I) - horse-radish peroxidase conjugate (100 micro l) were incubated at 4degree overnight or at 37degree for 2 h in the wells of a microtitre plate coated with rabbit anti-I antibodies. The wells were incubated with 5,5'- tetramethylbenzidine soln. (150 micro l) at 37degree in the dark for 30 min, the reaction was stopped by the addition of 6M-H2SO4 (50 micro l) and the absorbance was measured at 450 nm. Recoveries were quantitative. Detection limits were 4.8 and 5.1 micro g kg-1 of I in muscle and liver, respectively. Cross-reactivities (tabulated) were 0.1% with other sulphonamides except that for sulphamerazine which was 13.2%. Record 33 of 57
TI: Application of matrix solid-phase dispersion for the determination of clenbuterol in liver samples. AU: Boyd,-D; Shearan,-P; Hopkins,-JP; O'Keeffe,-M; Smyth,-MR AD: Natl. Food Centre, Dublin 15, Eire SO: Anal-Chim-Acta. 1 Apr 1993; 275(1-2): 221-226 AB: Liver was homogenized and mixed with [3H]clenbuterol. Portions (0.5 g) were mixed in a mortar with Bondesil C18 (40 micro m; 2 g). The mixture was transferred to a syringe containing two filter paper discs and the plunger was compressed to give a vol. of 4.5 ml. The material was washed with hexane (8 ml) and H2O (8 ml), the excess of solvent was removed by applying positive pressure and methanol (8 ml) was added. The first 1-ml portion of eluate was discarded, the remaining eluate was evaporated to dryness at 55degree under N and the residue was dissolved in ethanol (0.5 ml). Extracts (0.1 ml) were analysed by RIA carried out in tubes. Mixtures were evaporated to dryness at 40degree under N, phosphate - gelatin buffer soln. (0.5 ml) was added, the tubes were incubated at 37degree for 15 min and [3H]clenbuterol (0.1 ml) and antiserum (0.1 ml) were added. After incubation at 37degree for 15 min and overnight at 4degree, dextran - charcoal suspension (0.5 ml) was added and the tubes were centrifuged for 10 min at 1200 g. The supernatant soln. were decanted into phials and mixed with scintillation cocktail (10 ml) before liquid scintillation counting. The detection limit was 0.3 ng g-1 of clenbuterol in liver. Inter- and intra-assay coeff. of variation were 16.1 to 19.3 and 4.9 to 8.9%, respectively. Record 34 of 57
TI: Disruption and fractionation of biological materials by matrix solid-phase dispersion. AU: Baker,-SA; Long,-AR; Hines,-ME AD: Louisiana State Univ., Lab. Residue Stud., Dept. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Chromatogr. 15 Jan 1993; 629(1): 23-34 AB: A summary of data is presented on the application of matrix solid-phase dispersion to the isolation of drug and pollutant residues from a variety of biological matrices, and its application to the disruption and fractionation of muscle tissue, Mycobacterium paratuberculosis and Escherichia coli. Record 35 of 57
TI: Matrix solid-phase dispersion extraction and gas-chromatographic screening of 14 chlorinated pesticides in oysters (Crassostrea virginica). AU: Lott,-HM; Barker,-SA AD: Louisiana State Univ., Lab. Residue Stud., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-AOAC-Int. Jan-Feb 1993; 76(1): 67-72 AB: Oyster tissue, blended with delta-HCH as internal standard, was mixed with C18 silica and transferred to a bed of activated Florisil. The resulting column was compressed before elution of the pesticides with acetonitrile - methanol (9:1). A 2-micro l portion of the eluate was analysed by GC on a column (30 m x 0.25 mm) coated with DB-5 (0.2 micro m) and operated with temp. programming from 120degree (held for 2 min) at 10degree min-1 to 290degree (held for 4 min), N as carrier gas (15 cm s-1) and ECD. Peak area ratios were used for quantitation. Typical chromatograms obtained for oyster tissue fortified at 250 and 31.3 ng g-1 are reproduced, and recoveries and inter- and intra-assay variabilities are reported for 14 pesticides. The eluate from the extraction column was free from interfering co-extractives. Record 36 of 57
TI: Matrix solid-phase dispersion linked to immunoassay techniques for the determination of clenbuterol hydrochloride in bovine liver samples. AU: Boyd,-D; Shearan,-P; Hopkins,-JP; O'Keeffe,-M; Smyth,-MR AD: Natl. Food Centre, Dunsinea, Dublin 15, Eire SO: Anal-Proc (London). Mar 1993; 30(3): 156-157 AB: Clenbuterol hydrochloride (I) was extracted by blending the liver sample with C18 and solvent elution. The extracts were evaporated and the residues were dissolved in H2O for assay by using an enzyme immunoassay kit (Riedel-de Haen, Darmstadt, Germany) in which I competed with the I - peroxidase conjugate for binding to the antiserum and the final absorbance was measured at 410 nm. The kit had cross-reactivities of 71, 11, 10, 5.5 , 4.5 and 4% for mabuterol, salbutamol, terbutaline sulphate, cimaterol, carbuterol hydrochloride and isoprenaline, respectively. Recovery was satisfactory for 1 to 5 ng g-1 of added I, and results agreed well with those obtained by matrix solid-phase dispersion - RIA. Record 37 of 57
TI: Efficient biological analysis using MSPD [Matrix solid-phase dispersion]. AU: Barker,-S; Hawley-R AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. Toxicol. Sch. Vet. Med., Baton Rouge, LA, USA SO: Int-Lab. Sep 1992; 22(8): 46, 48 AB: Rapid and simple drug determinations and immuno- or receptor assays can be carried out using the matrix solid-phase dispersion technique for sample preparation. Samples are blended with C18 sorbent followed by elution of analytes from the sample - C18 matrix. This microscale
method minimizes the amount of solvents used and steps necessary for analysis. Its application to the determination of invermectin in beef liver is described. Record 38 of 57
TI: Liquid-chromatographic confirmatory method for five sulfonamides in salmon muscle tissue by matrix solid-phase dispersion. AU: Reimer,-GJ; Suarez,-A AD: CanTest Ltd., Vancouver, BC V6J IJ8, Canada SO: J-AOAC-Int. Nov-Dec 1992; 75(6): 979-981 AB: Salmon muscle tissue was extracted by matrix solid-phase dispersion (details given), the CH2Cl2 extracts were evaporated to dryness under N, the residue was washed with methanol, the soln. was evaporated to dryness and the residue was dissolved in 200 micro l of methanol. A 20- micro l portion of the soln. was analysed on a column (25 cm x 4.6 mm) of Supelcosil LC18-DB (5 micro m) with gradient elution with acetonitrile - 0.01M-ammonium acetate (pH 5.5) (details given) with photodiode array detection. Calibration graphs were rectilinear from 60 to 5000 ppb. Intra- assay coeff. of variation were generally 13% for sulfadiazine, sulfamerazine, sulfamethazine, sulfadimethoxine and sulfapyridine. Detection limits were 48 to 150 ppb. Average recoveries were 66 to 82%. Record 39 of 57
TI: Tissue drug residue extraction and monitoring by matrix solid-phase dispersion (MSPD) - HPLC analysis. AU: Barker,-SA; Long,-AR AD: Louisiana State Univ., Lab. Residue Studies, Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Liq-Chromatogr. Aug 1992; 15(12): 2071-2089 AB: A summary is given of the methodology of matrix solid-phase dispersion in cleanup of drug analytes extracted from tissues for determination by HPLC with UV or fluorimetric detection. The procedure involves use of a column of blended derivatized silica (solid-phase support) and tissue matrix for cleanup. The method is applied to several classes of drug. Record 40 of 57
TI: Matrix solid-phase dispersion isolation and liquid chromatographic determination of oxolinic acid in channel catfish (Ictalurus punctatus) muscle tissue. AU: Jarboe,-HH; Kleinow,-KM AD: Louisiana State Univ., Sch. Vet. Med., Dept. Vet. Physiol., Pharmacol. and Toxicol., Baton Rouge, LA 70803, USA SO: J-AOAC-Int. May-Jun 1992; 75(3): 428-432 AB: Muscle and bile containing piromidic acid (internal standard) were extracted on C18 columns. Oxolinic acid (I) and its metabolites were eluted by sequentially washing with acetonitrile and methanol. The eluates were combined, evaporated to dryness and the residue was reconstituted in 0.05M-acetic acid - methanol. A portion of the soln. was analysed by HPLC on a column (25 cm x 4.1 mm) of Versapack C18 (10 micro m) with gradient elution (1 ml min-1) with methanol and anhyd. 0.05M-acetic acid (details given) and detection at 260 nm. The calibration graph was rectilinear from 0.1 to 15 micro g g-1 of I and inter- and intra-assay coeff. of variation were 12.5 +/- 8.9 and 1.2%, respectively; recovery was 63 +/- 19.8 to 100.2 +/- 3.9%. The limit of detection was 0.05 micro g g-1. Record 41 of 57
TI: Matrix solid-phase dispersion extraction and liquid-chromatographic determination of nicarbazin in chicken tissue. AU: Schenck,-FJ; Barker,-SA; Long,-AR AD: US Food and Drug Admin., Baltimore, MD 21201, USA SO: J-AOAC-Int. Jul-Aug 1992; 75(4): 659-662 AB: A column packed with the tissue sample blended with C18 material was washed with hexane before nicarbazin was eluted with acetonitrile. After cleanup on alumina, it was determined on an Econosphere (3 micro m) column (15 cm x 4.6 mm) with detection at 340 nm. Recoveries were between 80.1 and 96.9% with coeff. of variation (n = 5) from 1.2 to 8.4%. The results are compared with those obtained by the conventional ethyl acetate extraction method. Record 42 of 57
TI: Matrix solid-phase dispersion extraction and liquid-chromatographic determination of ivermectin in bovine liver tissue. AU: Schenck,-FJ; Barker,-SA; Long,-AR AD: US Food and Drug Admin., Baltimore, MD 21201, USA SO: J-AOAC-Int. Jul-Aug 1992; 75(4): 655-658 AB: A column packed with a liver sample blended with C18 material was washed with hexane before elution of ivermectin with CH2Cl2 - ethyl acetate (3:1). After cleanup on alumina it was derivatized with DMF - acetic anhydride - 1-methylimidazole and determined on a column (25 cm x 4.6 mm) of Econosil C18 (5micro m) at 37degree with aq. 95% methanol as mobile phase (2 ml min-1) and fluorimetric detection at 418 nm (excitation at 364 nm). Recoveries were between 72.1 and 77.4% for samples treated with 10 to 40 ng g-1, with coeff. of variation (n = 5) from 7.3 to 12.9%. Record 43 of 57
TI: Analytical aspects of veterinary drug residues. AU: Haagsma,-N AD: Unvi. Utrecht, Dept. Sci. Food and Animal Origin, Fac. Vet. Med., 3508 TD Utrecht, Netherlands SO: Mikrochim-Acta. 1991; II(1-6): 63-70 AB: A review is presented, with 88 references, of recent developments in the determination of veterinary drug residues in food of animal origin. The application of solid-phase extraction, immunoaffinity and matrix solid-phase dispersion as rapid clean-up and concentration techniques is discussed. Automated methods, e.g., immunoassays and fully automated sample treatment LC, are also discussed. Record 44 of 57
TI: Determination of aminoglycoside antibiotics by reversed-phase ion-pair high-performance liquid chromatography coupled with pulsed amperometry and ion-spray mass spectrometry. AU: McLaughlin,-LG; Henion,-JD AD: Cornell Univ., Drug Testing and Toxicol., NYS Coll. Vet. Med., Ithaca, NY 14850, USA SO: J-Chromatogr. 7 Feb 1992; 591(1-2): 195-206 AB: Various stationary phases, mobile phase compositions and ion-pairing ions were evaluated for the cited detemination. Bovine tissues were extracted by matrix solid-phase dispersion as previously described (Schenck, US FDA Laboratory Information Bulletin, Vol. 7, Issue 4, No 3559). Best results were obtained by using a column (10 cm x 4.6 mm) of Spherisorb ODS-2 (3 micro m) with 8% acetontrile in 20mM-pentafluoropropionic acid as mobile phase. With pulsed amperometric detection at 0.1 V and a pulse duration of 480 ms, detection limits were in the ng range. For MS detection an ion-spray interface was used and MS was carried out with a triple quadrupole instrument equipped with an atmospheric pressure ion source in the positive ion mode. Selected-
ion monitoring was at m/e 351, 265, 301 and 293 for spectinomycin, hygromycin B, steptomycin and dihydrostrptomycin, respectively. Detection limits were in the low ng range. Record 45 of 57 ;
TI: Matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic screening of nine chlorinated pesticides in beef fat. AU: Long,-AR; Soliman,-MM; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. May-Jun 1991; 74(3): 493-496 AB: Beef fat (0.5 g) containing nine chlorinated pesticides (e.g., heptachlor, aldrin, dieldrin, endrin, pp'-DDT) and fortified with dibutyl chlorendate (internal standard; 25 micro g ml-1) was blended with 2 g of C18 (octadecylsilyl-derivatized silica; 40 micro m) and the homogeneous matrix blend was transferred to a column containing activated Florisil. The pesticides were eluted with 8 ml of acetonitrile and a 0.2-micro l portion of the eluate was analysed by GC on a column (25 m x 0.25 mm) of DB-5 (0.2 mm) with temp. programming from 120degree (held for 2 min) to 290degree (held for 2 min) at 10degree min-1, N as carrier gas (14 cm s-1) and ECD. Calibration graphs were rectilinear and mean intra- and inter-assay coeff. of variation were 2.5 to 5.1 and 6 to 14%, respectively. Recoveries ranged from 85 to 102% and co-extractants did not interfere. Record 46 of 57
TI: Multi-residue matrix solid-phase dispersion (MSPD) extraction and gas-chromatographic screening of nine chlorinated pesticides in catfish (Ictalurus punctatus) muscle tissue. AU: Long,-AR; Crouch,-MD; Barker,-SA AD: Louisiana State Univ., Sch. Vet. Med., Dept. Vet. Physiol., Pharmacol. and Toxicol., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. Jul-Aug 1991; 74(4): 667-670 AB: Fish muscle tissue (0.5 g) was blended into octadecylsilyl derivatized C18 silica (40 micro m) packing until homogenized. The blend was packed into a column containing 2 g of activated Florisil and pesticides were eluted with acetonitrile. A portion of the extract was analysed by GC on a column (25 m x 0.25 mm) of DB-5 (0.2 mm) with temp. programming from 120degree (held for 2 min) to 290degree (held for 5 min) at 10degree min-1, N as carrier gas (14 cm s-1) and ECD at - 0.24 mV. Calibration graphs were rectilinear and intra- and inter-assay coeff. of variation ranged from 1.8 to 4.7% and from 5.0 to 16.9%, respectively; recoveries were >=77.2%. A theoretical detection limit of ~10 ng g-1 was obtained by extrapolation of the data. Record 47 of 57
TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of furazolidone in pork muscle tissue. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. Mar-Apr 1991; 74(2): 292-294 AB: Pork muscle tissue (0.5 g) was homogenized with C18 (18% load; endcapped; 2 g). A column was made from the C18 - pork matrix which was washed with hexane (8 ml) before elution with ethyl acetate. The eluate was passed through a pre-washed activated alumina column and dried under N. The residue was mixed with 0.1 ml each of methanol and 0.015M-H3PO4 and the mixture was sonicated for 5 to 10 min then centrifuged at 17,000 g for 5 min. The clear supernatant was analysed by HPLC on a column (30 cm x 4 mm) of ODS (10 micro m), operated at 45degree, with a mobile phase (1 ml min-1) of 0.015M-H3PO4 - acetonitrile (3:2) and detection at 365 nm. The calibration graph was rectilinear and the average recovery was 89.5% for 7.8 to 250 ng g-1 of furazolidone. The detection limit was 390 pg and the inter- and intra-assay coeff. of variation were 9.9 and 1.5%, respectively. Record 48 of 57 ;
TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of sulphadimethoxine in catfish (Ictalurus punctatus) muscle tissue. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 868-871 AB: A 0.5-g portion of fish muscle tissue was blended with 2 g of C18 material (Analytichem International) and methanolic sulphamethoxazole (internal standard) and packed into a 10-ml column, followed by washing with hexane and elution with 8 ml of CH2Cl2. The eluate was evaporated at 40degree in a stream of N, and the residue was dispersed in 0.5 ml of mobile phase. The suspension was centrifuged and a portion (25 micro l) of the supernatant soln. was analysed by HPLC on a MicroPak ODS (10 micro m) column (30 cm x 4 mm) with a mobile phase (1 ml min- 1) of 17mM-H3PO4 - acetonitrile (13:7) and diode-array detection at 270 nm. Sulphadimethoxine and the internal standard were well separated, and calibration graphs of peak-area ratios were rectilinear up to 1.6 micro g g-1; the detection limit was 50 ng g-1. Record 49 of 57 ;
TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of oxytetracycline in catfish (Ictalurus punctatus) muscle tissue. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 864-867 AB: A 0.5-g portion of fish muscle tissue was blended with a mixture of 2 g of C18 material (Analytichem International) and 0.05 g each of EDTA and oxalic acid and packed into a 10-ml column, followed by washing with hexane and elution of oxytetracycline (I) with 8 ml of 0.06% t- butyl-4-methoxyphenol - 0.06% 2,6-di-t-butyl-p-cresol in acetonitrile - methanol (1:1). The eluate was evaporated at 40degree in a stream of N, and the residue was dispersed in 0.5 ml of mobile phase. The suspension was centrifuged and the supernatant soln. (25 micro l) was injected on to a MicroPak ODS (10 micro m) column (30 cm x 4 mm) with a mobile phase (1 ml min-1) of 0.02M- oxalic acid - acetonitrile - methanol (28:11:1) and diode-array detection at 365 nm. Calibration graphs of peak area were rectilinear up to 3.2 micro g g-1 of I; the detection limit was 50 ng g-1. Record 50 of 57 ;
TI: Matrix solid-phase dispersion isolation and liquid-chromatographic determination of five benzimidazole anthelmintics in fortified beef liver. AU: Long,-AR; Malbrough,-MS; Hsieh,-LC; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. Nov-Dec 1990; 73(6): 860-863 AB: A 0.5-g portion of liver was added to 2 g of C18 material (Analytichem International), a mixture of albendazole, fenbendazole, oxfendazole, thiabendazole and mebendazole (internal standard) was added. The mixture was blended, packed into a 10-ml column,followed by washing with hexane and elution of the benzimidazoles with 8 ml of acetonitrile. The eluate was purified by passage through an alumina column and evaporated in a stream of N, and the residue was dispersed in 0.1 ml of methanol plus 0.4 ml of 17mM-H3PO4. The suspension was centrifuged, the supernatant soln. was filtered (0.45 micro m), and a 20-micro l portion of the filtrate was injected on to a MicroPak ODS (10 micro m) column (30 cm x 4 mm) operated with 17mM-H3PO4 - acetonitrile (3:2) as mobile phase (1 ml min-1) and diode-array detection at 290 nm. The calibration graphs of peak area were rectilinear up to 3.2 micro g g-1 of the four analytes; the detection limit was 0.1 micro g g-1. Record 51 of 57
TI: Quantitative method for the detection of sulphonamide residues in meat and milk samples with a high-performance thin-layer-chromatographic method. AU: Van-Poucke,-LSG; Depourcq,-GCI; Van-Peteghem,-CH AD: State Univ. Ghent, Lab. Pharm. Microbiol. and Hyg., 9000 Ghent, Belgium SO: J-Chromatogr-Sci. Oct 1991; 29(10): 423-427 AB: A high-performance TLC method for the separation and detection of sulphonamides after solid-phase extraction for meat samples and a modified matrix solid-phase dispersion extraction for milk is described. The extracts were applied to Kieselgel 60 F254 plates which were developed for 30 min in a saturated chamber with a three-multiple development system with methanol (containing 2% ammonia) - CH2Cl2 (30:70, 15:85 and 5:95) to successive distances of 15, 30 and 45 mm, respectively. The calibration graph was rectilinear for 0.5 to 40 mg of the six sulphonamides tested; the limit of quantification was 4 micro g kg-1. Record 52 of 57
TI: Veterinary drug residues in meat - possibilities of their analytical determination. AU: Petz,-M AD: Bergische Univ. GH, Lehrstuhl Lebensmittelchem., 5600 Wuppertal, Germany SO: Mitt-Geb-Lebensmittelunters-Hyg. 1991; 82(1): 7-23 AB: A review is presented, with 43 references. The most recently proposed limits for veterinary drugs in animal tissues, milk and eggs (FAO/WHO 1990) are tabulated and the results of recent surveys are discussed. Suitable screening tests and methods of determination are described. Newer methods of separation from the matrix, e.g., matrix solid-phase dispersion, immunoaffinity chromatography, are given special attention. Record 53 of 57
TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of clorsulon in milk. AU: Schenck,-FJ; Barker,-SA; Long,-AR AD: Food and Drug Admin., Baltimore, MD 21201, USA SO: J-Liq-Chromatogr. Sep 1991; 14(15): 2827-2834 AB: Milk (0.5 g) was blended with C18 packing material (2 g) and the mixture was loaded into an empty syringe barrel fitted with a frit. The column was washed with hexane (3 ml), the eluate was discarded and the column was attached to a Florisil solid phase extraction cartridge. The tandem columns were eluted with ethyl ether (3 x 3 ml), the C18 column was removed and clorsulon (I) was eluted from the Florisil column with 2 ml of ether. The eluate was evaporated to dryness, the residue was dissolved in mobile phase (1 ml) and the soln. was filtered. A portion (200 micro l) of the filtrate was analysed by HPLC on a column (15 cm x 4.6 mm) of Econosphere (3 micro m) with a mobile phase (1 ml min-1) of acetonitrile - phosphate buffer soln. of pH 7 (1:3) and detection at 265 nm. Recoveries were 88.8 to 96.6% for 50 to 200 ppm of I with coeff. of variation of 2.7 to 7.9%. Record 54 of 57
TI: Matrix solid-phase dispersion (MSPD) extraction and liquid-chromatographic determination of five benzimidazole anthelmintics in pork muscle tissue. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol. Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Food-Compos-Anal. Mar 90; 3(1): 20-26 AB: Tissue was blended (1:4) with 18% ODS silica (40 micro m) and the blend was packed into a 10-ml plastic syringe barrel and washed with hexane before elution of albendazole (I), fenbendazole (II), oxfendazole (III) and thiabendazole (IV) with acetonitrile. The eluate was cleaned up by passage through a column of activated alumina and a portion was analysed by
HPLC on a column (30 cm x 4 mm) of ODS silica (10 micro m) at 45degree with aq. 17mM-H3PO4 - acetonitrile (3:2) as mobile phase (1.0 ml min-1) and detection at 290 nm vs. mebendazole as internal standard. Recoveries of 0.1 to 3.2 mg g-1 were 86 to 104% for I, 92 to 105% for II, 78 to 101% for III and 73 to 93% for IV, with mean coeff. of variation of 6.4, 5.5, 7.9 and 7.2%, respectively. Record 55 of 57
TI: Matrix solid-phase dispersion (MSPD) isolation and liquid-chromatographic determination of oxytetracycline, tetracycline and chlortetracycline in milk. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol. Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Assoc-Off-Anal-Chem. May-Jun 1990; 73(3): 379-384 AB: Milk (0.5 ml) was mixed with 2 g of C18 silica, 0.05 g of Na2EDTA and 0.05 g of oxalic acid, with gentle grinding to give a homogeneous mixture. The resulting material was packed into a column (10-ml plastic syringe) and washed with hexane (8 ml). The cited drugs were eluted with ethyl acetate - acetonitrile (1:3; 8 ml), the solvent was evaporated, and the residue was dissolved in mobile phase for HPLC analysis. This was performed on a column (30 cm x 4 mm) of Micro Pak ODS (10 micro m), with 10mM-oxalic acid - acetonitrile (7:3) at 40degree as mobile phase (1 ml min-1) and detection at 365 nm. Calibration graphs were rectilinear for 100 to 3200 ng ml-1, and recoveries were 63.5 to 93.3%. Inter- and intra-assay coeff. of variation (n = 5) were 8.5 to 20.7% and 1.0 to 9.3%, respectively. Record 56 of 57 ;
TI: Method for the isolation and liquid-chromatographic determination of chloramphenicol in milk. AU: Long,-AR; Hsieh,-LC; Bello,-AC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisiana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Agric-Food-Chem. Feb 1990; 38(2): 427-429 AB: A modification of the matrix solid-phase dispersion extraction method of Barker et al. (Anal. Abstr., 1990, 52, 5D21) was applied in the determination of chloramphenicol (I) in cow`s milk. The extracts were analysed by HPLC on a Varian MCH-10 (10 micro m) column (30 cm x 4 mm) at 35degree with 17mM-H3PO4 - acetonitrile (13:7) as mobile phase (1 ml min-1) and photodiode- array detection at 278 nm. The calibration graph was rectilinear from 62.5 to 2000 ng ml-1 of I and recoveries were from 60.8 to 79.0%. Inter- and intra-assay coeff. of variation were 11.6 (n = 30) and 1.4% (n = 5), respectively. Record 57 of 57 ;
TI: Multi-residue method for the determination of sulphonamides in pork tissue. AU: Long,-AR; Hsieh,-LC; Malbrough,-MS; Short,-CR; Barker,-SA AD: Louisana State Univ., Dept. Vet. Physiol., Pharmacol. and Toxicol., Sch. Vet. Med., Baton Rouge, LA 70803, USA SO: J-Agric-Food-Chem. Feb 1990; 38(2): 423-426 AB: A modification of the matrix solid-phase dispersion extraction method of Barker et al. (Anal. Abstr., 1990, 52, 5D21) with CH2Cl2 as eluent was applied in the determination of sulphadiazine, sulphadimethoxine, sulphadimidine, sulphafurazole, sulphamethizole, sulphanilamide and sulphathiazole in pork (0.5 g). The extracts were analysed by HPLC on a Varian MCH-10 column (30 cm x 4 mm) at 40degree with 17mM-H3PO4 - acetonitrile (7:3) as mobile phase (1 ml min-1) and photodiode-array detection at 270 nm. Sulfamerazine was used as internal standard. Calibration graphs were rectilinear from 62.5 to 2000 ng g-1 of each sulphonamide and detection limits were from 31.3 to 62.5 ng g-1. Inter- and intra-assay coeff. of variation were 7.2 to 13.3% (n = 30) and 3.5 to 6.2% (n = 5), respectively. Recoveries were from 70.4 to 95.8%. The method is simple, yields interference-free extracts and may be applied to other tissues or matrices.
WASHOE COUNTY SCHOOL DISTRICT Reno, Nevada REGULAR MEETING OF THE BOARD OF TRUSTEES April 3, 2012 TITLE: Presentation and Approval of the Fiscal Year 2012-13 Tentative Budget FROM: Mike Schroeder, Interim Chief Financial Officer PRESENTER(S) & PRESENTATION TIME: Mike Schroeder, Interim Chief Financial Officer (15 minutes) DATE REPORT WRITTEN: March 30, 2012