Gas-Liquid Chromatographic Determination of Captan and Two Metabolites in Milk and Meat

1977 ◽  
Vol 60 (3) ◽  
pp. 679-681
Author(s):  
John H Onley
Keyword(s):  
Ethyl Acetate ◽  
Silica Gel ◽  
Chromatographic Determination ◽  
Gel Chromatography ◽  
Milk Samples ◽  
Liquid Chromatographic Determination ◽  
Meat Samples ◽  
Silica Gel Chromatography ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) method has been developed for the determination of captan (N-trichloromethylthio-4-cyclohexene-1, 2-dicarboximide) and 2 metabolites, tetrahydrophthalimide (THPI) and tetrahydrophthalamic acid (THPMA), in milk and meat. The sample is extracted with ethyl acetate and is cleaned up by acetonitrile partition and silica gel chromatography where captan, THPI, and THPMA are separated. Captan is directly determined by GLC. THPI and THPMA are separately derivatized in an acetone solution of penta fluorobenzyl bromide. The resultant derivatives are purified separately on an Al2O3, column and quantitated by GLC, using an electron capture detector. Recoveries from milk samples fortified at 0.02–10 ppm ranged from 71 to 102%; recoveries from meat samples fortified at 0.04–10 ppm ranged from 75 to 99%.

scholarly journals Liquid Chromatographic Determination of the Processing Aid 4-Hexylresorcinol in Shrimp

1991 ◽  
Vol 74 (6) ◽  
pp. 1003-1005 ◽  
Author(s):  
Joan M King ◽  
Arthur J McEvily ◽  
Radha Iyengar
Keyword(s):  
Standard Deviation ◽  
Ethyl Acetate ◽  
Chromatographic Determination ◽  
Uv Detection ◽  
Liquid Chromatographic Determination ◽  
Meat Samples ◽  
Liquid Chromatographic

Abstract A rapid, sensitive, liquid chromatographic (LC) method has been developed for determination of residuals of the processing aid, 4-hexylresorcinol, on shrimp meat. An aqueous homogenate of shrimp meat is extracted with ethyl acetate followed by precolumn preparation on a silica Sep-Pak cartridge. LC determination is preformed with a Nova-Pak C18 column, with UV detection at 214 nm. Sensitivity was 0.006 μg, and recovery from shrimp meat samples of known 4-hexylresorcinol addition was 94%. Shrimp treated with 4-hexylresorcinol under the recommended dip protocol had mean residuals of 1.18 ppm, with a standard deviation of 0.13 ppm.

Liquid Chromatographic Determination of Rotenone in Fish, Crayfish, Mussels, and Sediments

1988 ◽  
Vol 71 (6) ◽  
pp. 1094-1096
Author(s):  
Verdel K Dawson ◽  
John L Allen
Keyword(s):  
Silica Gel ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Fish Muscle ◽  
Gel Chromatography ◽  
Tissue Samples ◽  
Sediment Samples ◽  
Liquid Chromatographic Determination ◽  
Silica Gel Chromatography ◽  
Liquid Chromatographic

Abstract An analytical procedure is described for determining residues of rotenone in fish muscle, fish offal, crayfish, freshwater mussels, and bottom sediments. Tissue samples were extracted with ethyl ether and extracts were cleaned up by gel permeation chromatography and silica gel chromatography. Sediment samples were extracted with methanol, acidified, partitioned into hexane, and cleaned up on a silica gel column. Rotenone residues were quantitated by liquid chromatography, using ultraviolet (295 nm) detection. Recoveries from sediment samples fortified with rotenone at 0.3 μg/g were 80.8%, whereas recoveries from tissue samples fortified with 0.1 μg/g ranged from 87.7 to 96.8%. Samples fortified with 0.3 μg/g and stored at - 10°C for 6 months before analysis had recoveries ranging from 83.2 to 90.5%. Limits of detection were 0.025 μg/g for sediments and 0.005 μg/g for tissue samples

Collaborative Study of the Quantitative Gas-Liquid Chromatographic Determination of Fusel Oil and Other Components in Whisky

1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger
Keyword(s):  
Ethyl Acetate ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Official Method ◽  
Fusel Oil ◽  
Fusel Alcohols ◽  
Aoac Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.

Modified Method for Electron Capture Gas-Liquid Chromatographic Determination of Diethylstilbestrol Residues in Urine of Fattened Bulls

1983 ◽  
Vol 66 (5) ◽  
pp. 1230-1233
Author(s):  
Athanasios E Tirpenou ◽  
Stylianos D Kilikidis ◽  
Athanasios P Kamarianos
Keyword(s):  
Sodium Hydroxide ◽  
Electron Capture ◽  
Silica Gel ◽  
Chromatographic Determination ◽  
Trifluoroacetic Anhydride ◽  
Phenolic Fraction ◽  
Modified Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) method with electron capture (EC) detection was developed fof determining diethylstilbestrol residues in the urine of fattened bulls. Diethylstilbestrol (DES) is extracted into benzene, and then into IN sodium hydroxide. The pH of the phenolic fraction (alkaline phase) is adjusted to 10.2 and DES is extracted again into benzene. Sample extracts are cleaned up on silica gel. Trifluoroacetic anhydride (TFAA) is used as acylation reagent, and the derivatized sample is chromatographed on a 3% OV-17 column and measured with a 63Ni EC detector. The method is suitable for determining residues at levels as low as 2 ppb.

Isolation, Purification, and Liquid Chromatographic Determination of Stilbene Phytoalexins in Peanuts

1995 ◽  
Vol 78 (5) ◽  
pp. 1177-1182 ◽  
Author(s):  
Victor S Sobolev ◽  
Richard J Cole ◽  
Joe W Dorner ◽  
Boris Yagen
Keyword(s):  
Acetic Acid ◽  
Silica Gel ◽  
Mobile Phase ◽  
High Speed ◽  
Chromatographic Determination ◽  
Normal Phase ◽  
Phase Partition ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method for determination of stilbene phytoalexins (SPs) in peanuts has been developed. SPs were extracted with acetonitrile–water (90 + 10, v/v) by high-speed blending. An aliquot of extract was applied to a minicolumn packed with AI2O3–ODS (C18) mixture and eluted with acetonitrile-water (90 + 10, v/v). Eluate was evaporated under nitrogen, and residue was dissolved in LC mobile phase. SPs in an aliquot of purified extract were quantitated by normal-phase partition LC on silica gel with n-heptane–2-propanol–water–acetonitrile–acetic acid (1050 + 270 + 17 + 5 + 1, v/v) as mobile phase. Recoveries of SPs [frans-4-(3-methyl-but-1-enyl)-3,5,4′-trihy-droxystilbene (trans-arachidin-3; t-Ar-3), trans-3-isopentadienyl-4,3′,5′-trihydroxystilbene (t-IPD), and trans-3,5,4′-trihydroxystilbene (trans-resveratrol; t-Res)] from peanuts spiked at 300 ppb were 96.05 ± 2.8%. Limits of quantitation for t-Ar-3 and t-IPD were about 100 ppb. t-Ar-3, t-IPD, and t-Res were found in all parts of the peanut plant as major SPs produced in response to fungal invasion.

Liquid Chromatographic Determination of Simazine, Atrazine, and Propazine Residues in Catfish

1995 ◽  
Vol 78 (4) ◽  
pp. 1067-1071 ◽  
Author(s):  
David C Holland ◽  
Robert K Munns ◽  
José E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long
Keyword(s):  
Ethyl Acetate ◽  
Petroleum Ether ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Triazine Herbicides ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the simultaneous determination of the triazine herbicides, simazine (SIM), atrazine (ATZ), and propazine (PRO) in the 12.5–100 ppb range in catfish. The herbicides are extracted from catfish homogenates with ethyl acetate, followed by solvent partitioning between acetonitrile and petroleum ether and additional cleanup on a C18 cartridge. A Supelcosil LC-18-DB column is used for LC separation, and UV determination is at 220 nm. The isocratic mobile phase is a mixture of methanol, acetonitrile, and water. Mean recoveries from catfish were 88.7, 96.9, and 91.7%; standard deviations were 6.84,7.78, and 6.26%; and coefficients of variation were 7.72,8.03, and 6.82% for SIM, ATZ, and PRO, respectively.

scholarly journals Liquid Chromatographic Determination of Tylosin in Mastitic Cow's Milk Following Therapy

1999 ◽  
Vol 82 (6) ◽  
pp. 1303-1307 ◽  
Author(s):  
Eva Dudriková ◽  
Sokol Jozef ◽  
Nagy Jozef
Keyword(s):  
Chromatographic Analysis ◽  
Chromatographic Determination ◽  
Maximum Residue Limit ◽  
Withdrawal Time ◽  
Milk Samples ◽  
Final Treatment ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Liquid chromatographic analysis of milk samples from 6 cows treated with tylosin in a veterinary practice indicated that tylosin persisted in milk for more than 3 days after the final treatment. The concentration of tylosin was not below the stated maximum residue limit (0.05 mg/kg). The milk from 3 cows being treated for mastitis catarrhalis chronica contained tylosin residues for 3.5 days after the last withdrawal time (72 h). No residue was detected in the milk of any animal 6 days after cessation of therapy.

Liquid Chromatographic Determination of Depletion of Bithionol Sulfoxide and Its Two Major Metabolites in Bovine Milk

1987 ◽  
Vol 70 (5) ◽  
pp. 810-812
Author(s):  
Dominique Mourot ◽  
MichÈle Dagorn ◽  
Bernard Delepine
Keyword(s):  
Bovine Milk ◽  
Chromatographic Determination ◽  
Milk Samples ◽  
Lactating Cows ◽  
Holstein Friesian ◽  
Liquid Chromatographic Method ◽  
Reliable Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method is described for determining bithionol sulfoxide and its metabolites, bithionol and bithionol sulfone, in milk. Samples are treated with HC1 to precipitate proteins and to permit extraction of bithionol sulfoxide in nonionized form. Tetrahydrofuran is added to the organic phase to facilitate extraction in diethyl ether; the dried residue is dissolved in chloroform, hexane, and sodium hydroxide and subjected to LC analysis. Residues of bithionol sulfoxide and its 2 metabolites were determined in milk of lactating cows. Holstein-Friesian dairy cows were administered a single oral dose of bithionol sulfoxide (50 mg/kg). Milk samples were analyzed with a reliable detection level of 0.025 pg/mL for each compound. Residues of bithionol sulfoxide and bithionol were detected during 30 and 16 milkings, respectively; bithionol sulfone was never present at detectable levels

Sign in / Sign up

Export Citation Format

Share Document