Evidence for Transformation of Sulfamethazine to its N4-Glucopyranosyl Derivative in Swine Liver During Frozen Storage

1984 ◽  
Vol 67 (3) ◽  
pp. 566-569 ◽  
Author(s):  
Owen W Parks

Abstract An analytical procedure for determining N4-glucopyranosylsulfamethazine (GPS) in swine livers is described. The sulfamethazine derivative is extracted from the tissues with water. GPS is isolated in sufficient purity for liquid chromatographic determination by a series of adsorption chromatographic procedures. Recovery of the conjugate from spiked swine livers was 82.2% with a coefficient of variation of 4.5%. Evidence is presented suggesting that sulfamethazine in swine livers is transformed to GPS during frozen storage. Two samples of swine liver in which incurred sulfamethazine residues were substantially depleted during frozen storage were analyzed for GPS. The conjugate accounted for 96.2% and 92.2% of the depleted sulfamethazine residues.

1983 ◽  
Vol 66 (3) ◽  
pp. 801-803
Author(s):  
Margie E Owen ◽  
◽  
O O Bennett ◽  
L T Chenery ◽  
C J Cohen ◽  
...  

Abstract A method for analyzing fensulfothion was tested by 10 collaborators. Formulations were dissolved, or extracted from inerts, in methanol. Benzophenone was used as an internal standard. The solution was diromatographed on a Partisil-10 ODS-2, or equivalent, reverse phase column, and detected at 230 nm. A mobile phase of methanol-water-phosphoric acid was used. The ratio of fensulfothion peak height to benzophenone peak height was calculated from the UV response and compared to the standard material for quantitation. A 15% granular formulation was analyzed as a matched pair. The results of one collaborator were outliers by the Dixon test. The coefficient of variation for the granular formulation was 1.6%. A matched pair of 63% spray concentrate samples was analyzed by 10 collaborators. The difference in results was an outlier for one collaborator; the coefficient of variation for the other collaborators was 1.5%. The method has been adopted official first action.


1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.


1983 ◽  
Vol 66 (2) ◽  
pp. 284-286
Author(s):  
Thomas D Macy ◽  
Andrew Loh

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine monensin in feed premixes. The method is simple and rapid. Monensin is extracted with methanol-water and determined in the extracting solution by HPLC. Average recovery for monensin from a 13.2% premix sample was 103% (coefficient of variation (CV), 2.6%) by HPLC and compares with the value of 100% (CV, 3.4%) obtained by the turbidimetric bioassay method.


2012 ◽  
Vol 10 (5) ◽  
pp. 1459-1463 ◽  
Author(s):  
Paraskevas Tzanavaras ◽  
Theano Karakosta ◽  
Pantelis Rigas ◽  
Demetrius Themelis ◽  
Anastasia Zotou

AbstractThe first HPLC method for the separation of three paraben preservatives (methyl-, ethyl- and propyl parabens) using a core-shell analytical column is reported in this study. The separation was completed in less than 8 min at a low flow rate of 0.4 mL min−1 and an isocratic mobile phase containing 20% acetonitrile as organic modifier. The backpressure was HPLC equipment. The proposed analytical procedure was validated for linearity (0.5–20 µg L−1), limits of detection (15–43 µg L−1) and quantification (50–142 µg L−1), selectivity, within day (1.3–1.5%) and day-to-day (3.4–4.6%) precision and accuracy. The proposed method has been applied to the determination of the selected paraben preservatives in commercially available hygiene wipes. The mean percent recoveries were found to be in the range of 98.0–98.4%.


1988 ◽  
Vol 71 (3) ◽  
pp. 480-484 ◽  
Author(s):  
Michel R Lapointe ◽  
Huguette Cohen

Abstract A high-speed liquid chromatographic (LC) method using post-column derivatization is described for the determination of monensin, narasin, and salinomycin in a variety of animal feeds. The ionophores are extracted with hexane-ethyl acetate (90 + 10). A portion of the sample is evaporated, diluted to a known volume, and analyzed using a 6 cm 3 μm C18 column and an absorbance detector after post-column reaction with vanillin. The method has been applied to poultry and swine feeds with levels of 3-100 ppm added antibiotic. A comparison was also carried out with medicated poultry feed and beef feed lot supplement samples previously analyzed by 2 separate bioassay methods for monensin and salinomycin, respectively. Recoveries for the LC method ranged from 92.1 to 103% with an average recovery of 98.1% and a coefficient of variation of 3.65%.


1990 ◽  
Vol 73 (1) ◽  
pp. 51-53
Author(s):  
James B Noffsinger ◽  
Martha Emery ◽  
Daniel J Hoch ◽  
Jarmila Dokladalova

Abstract A liquid chromatographic (LC) method has been developed to determine the content of polydextrose, a water-soluble 1 calorie/g bulking agent, in food matrixes such as cookies, cakes, fruit spreads, and chocolate toppings. This analysis, which requires use of a blank matrix, provides a feasible means to control the manufacture of foods containing this additive and provides a component for the accurate determination of the caloric value of a particular food product. The method involves aqueous extraction of the polydextrose from the food matrix followed by separation on a carbohydrate analysis column. The LC system uses a mobile phase of 0.005M CaS04*2H2o and a refractive index detector for quantitation. Polydextrose recoveries from the food matrixes varied from 91.5 to 100.9% with assay precision, expressed as coefficient of variation, ranging from 0.7 to 4.3%. Each error estimate was derived from 5 parallel determinations. The present methodology is precise and selective in contrast to the modified classical phenol-sulfuric acid colorimetric method for assaying carbohydrates, which had been used for polydextrose determination in food matrixes in the past. Because the coefficient of variation frequently exceeded 10%, replicate analyses were necessary to achieve quantitation.


1970 ◽  
Vol 16 (7) ◽  
pp. 587-593 ◽  
Author(s):  
H E Sine ◽  
M J McKenna ◽  
T A Rejent ◽  
M H Murray

Abstract A method is presented for the rapid gas chromatographic determination of barbiturates and glutethimide in serum, suitable for use in clinical emergencies. The sample is prepared for gas chromatography by acidification and a single extraction with chloroform. From 70 to 100% of the various barbiturates and glutethimide are analytically recovered, with a coefficient of variation of 8 to 10% for the method. During a 10-month clinical evaluation (87 requested determinations), 34 analyses (39% of the samples submitted) were positive for barbiturates, glutethimide, or both.


1978 ◽  
Vol 61 (5) ◽  
pp. 1070-1073
Author(s):  
Robert B Hagel

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine lasalocid in premixes. The method is simple and rapid, requiring an extraction of the drug and separation of insoluble material before HPLC. Elution times are typically <10 min per sample. The average recoveries for lasalocid at the 16.5 and 50% levels were 100.2±2 and 100.0±2%, respectively. The precision of the method (coefficient of variation = 0.02) compares favorably with that of the approved bioassay (coefficient of variation = 0.06).


1991 ◽  
Vol 74 (5) ◽  
pp. 780-784 ◽  
Author(s):  
David C Holland ◽  
Kent C Faul ◽  
Jose E Roybal ◽  
Robert K Munns ◽  
Wilbert Shimoda

Abstract A liquid chromatographic (LC) method is described for the determination of chlortetracycline hydrochloride (CTC) in poultry/swine and ruminant feeds in the 10-100 ppm range and in premix. CTC is extracted from ground feed/premix with acidified acetone, and the extract is filtered through a Millex-HV filter or disposable C 18 column. The filtrate Is partitioned with methylene chloride when additional cleanup is necessary. A Nova-Pak C 18 column Is used for LC separation with determination at 370 nm. The average recovery of CTC from premix was 95% with a standard deviation (SD) of 1.70 and a coefficient of variation (CV) of 1.79%. The overall average recovery from feeds was 77% with an SO of 3.18 and a CV of 4.10%.


1990 ◽  
Vol 73 (3) ◽  
pp. 368-373 ◽  
Author(s):  
Susan S.-C Tai ◽  
Nancy Cargile ◽  
Charlie J Barnes

Abstract The liquid chromatographic determination previously developed for benzlmldazoles in cattle liver has been slightly modified and applied to the determination of 4 benzlmldazoles In milk. Recoveries of fenbendazole (FBZ), oxfendazole (OFZ), and thiabendazole (TBZ) from milk fortified at the 10 ppb level were 80% or greater with an Intralaboratory coefficient of variation of 11 % or less. Recovery of 5-hydroxythiabendazole (5-OH-TBZ) at the 30 ppb level averaged 56% with an Intralaboratory coefficient of variation of 5%. Limited data on the depletion of FBZ, OFZ, TBZ, and 5-OHTBZ In milk were also generated.


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