Liquid Chromatographic Determination of Fumonisins B1, B2, and B3 in Foods and Feeds

1992 ◽  
Vol 75 (2) ◽  
pp. 313-318 ◽  
Author(s):  
Eric W Sydenham, ◽  
Gordon S Shephard, ◽  
Peter G Thiel

Abstract Three recently described and toxlcologlcally Important Fusarlum mycotoxins, fumonisln B1 (FB1), fumonisln B2 (FB2), and fumonisln B3 (FB3), are the major fumonisins produced In cultures of F. monlllforme, a fungus that occurs worldwide on corn. Contamination of food and feed with F. monlllforme has been associated with a number of diseases In both animals and humans. Aspects of a recently reported liquid chromatographic method for the determination of FB1 and FB2 in corn, including Initial extraction, extract purification, and stability of derivatives, were Investigated and, where necessary, optimized further both to reduce the analysis time and to include the co-determlnatlon of FB3. The method was applied for the determination of FB3, in a series of U.S. feed samples associated with outbreaks of equine leukoencephalomalacla, which were shown previously to contain both FBi and FB2. Twelve of the 13 feed samples contained FB3 at levels ranging between 50 and 2650 ng/g, corresponding to 2.2-18% of the total fumonisln concentrations present in the FB3-posltlve feed samples. This is the first report of the natural occurrence of FB3.

1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.


1984 ◽  
Vol 67 (3) ◽  
pp. 497-499
Author(s):  
Stephen C Slahck ◽  
◽  
J B Audino ◽  
O O Bennett ◽  
B D Folsom ◽  
...  

Abstract A liquid chromatographic method for the determination of propoxur in technical and formulated products has been subjected to a collaborative study with 8 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with n-butyrophenone as an internal standard. Collaborators were furnished with samples of technical, 70% wettable powder, 1.5 emulsifiable, and 2% bait. Coefficient of variation values obtained on the 4 samples were 0.34, 0.68, 3.25, and 5.41%, respectively. The method has been adopted official first action.


1988 ◽  
Vol 71 (1) ◽  
pp. 36-37
Author(s):  
Ramesh J Trivedi

Abstract A simple, sensitive, and rapid liquid chromatographic method for quantitating α-ionone in toothpaste at levels of 20 ppm in the presence of large amounts of flavor has been developed. The method is accurate, precise, cost-effective, and specific for α-ionone. Average recovery of a laboratory-prepared sample was 99.0% with the relative standard deviation was 1.29% (n = 6).


1975 ◽  
Vol 58 (1) ◽  
pp. 48-49 ◽  
Author(s):  
Manjeet Singh

Abstract A high-pressure liquid chromatographic method is presented for the isolation and determination of uncombined intermediates and subsidiary colors in FD&C Blue No. 2 (indigotine, C.I. No. 73015). Samples of FD&C Blue No. 2 containing 0.1–0.3% isatin, 0.1–0.3% isatin 5-sulfonic acid, 0.1–5.0% monosulfonated indigo, and 1.0–18.0% 5,7’-disulfonated indigo were prepared and analyzed by using this method. Recoveries ranged between 92 and 102%.


1976 ◽  
Vol 59 (3) ◽  
pp. 708-710
Author(s):  
Alan R Hanks ◽  
Christine W Cramer

Abstract A gas-liquid chromatographic method has been developed to determine pentachloronitrobenzene (PCNB) in pesticide formulations including dusts, powders, granules, liquids, and fertilizers. Captan, disulfoton, and Terrazole do not interfere. Samples are extracted with chloroform, and an aliquot is mixed with an equal volume of internal standard solution containing o-terphenyl. PCNB is chromatographed on a 5% SE-30 column and quantitated by peak height ratios. The method has been subjected to a ruggedness test which indicates little sensitivity to changes in extraction and chromatographic conditions.


1988 ◽  
Vol 71 (5) ◽  
pp. 1054-1056 ◽  
Author(s):  
Joel E Houglum ◽  
Richard D Larson ◽  
Rose M Neal

Abstract A reverse-phase liquid chromatographic method for the assay of sulfamethazine (SMZ) in feeds is described. Feed samples are extracted with 50% methanol solution, centrifuged, filtered, and diluted when necessary, and chromatographed on a C-18 column. Samples are eluted with a mobile phase of 20% methanol and 80% of a solution containing acetic acid and tetramethylammonium chloride. The average recovery from spiked samples was 97.2% with a coefficient of variation of 1.2%. Linearity was very good (correlation coefficient 0.9997). Within-day and between-day coefficients of variation averaged 1.3 and 2.6%, respectively. The results for samples assayed by this method compared closely with the results from the same extracts assayed by the AOAC colorimetric method


1984 ◽  
Vol 67 (6) ◽  
pp. 1118-1120
Author(s):  
Ting Susan ◽  
◽  
R L Brown ◽  
L A Dougherty ◽  
J B Schepman ◽  
...  

Abstract A reverse phase liquid chromatographic method for the determination of methyldopa, methyldopa-hydrochlorothiazide, and methyldopachlorothiazide in tablets was collaboratively studied by 8 laboratories. Each collaborator received 20 samples that included drug substance, synthetic and commercial tablet compositions. The overall repeatability and reproducibility standard deviations for commercial tablets were 1.11 and 1.75% for methyldopa, 0.96 and 1.62% for chlorothiazide, and 1.21 and 2.15% for hydrochlorothiazide, respectively. The overall recoveries of methyldopa, chlorothiazide, and hydrochlorothiazide added to synthetic tablets were 100.78, 100.70, and 101.34%, respectively. The method has been adopted official first action.


1993 ◽  
Vol 76 (5) ◽  
pp. 1143-1145 ◽  
Author(s):  
Mei-Chich Hsu ◽  
Weng F Huang

Abstract A previously published liquid chromatographic method proposed for the analysis of dicloxacillin preparations was subjected to an interlaboratory study. The method is rigorously defined in terms of performance requirements, yet allows a degree of flexibility to the individual analyst. Eight laboratories participated in a study to analyze 3 samples in duplicate. Estimates for the repeatability and reproducibility of the method, expressed as relative standard deviations of the results of the determination of dicloxacillin preparations, were <0.57 and 2.56%, respectively.


1987 ◽  
Vol 33 (12) ◽  
pp. 2278-2280 ◽  
Author(s):  
G Severini ◽  
L M Aliberti

Abstract We used a liquid-chromatographic method to measure xanthine, hypoxanthine, and inosine in plasma of uremic patients before and after hemodialysis. The concentrations of all three were higher than in normal subjects. After dialysis treatment, the values were significantly lower than before dialysis, but still above normal.


1988 ◽  
Vol 71 (3) ◽  
pp. 528-530 ◽  
Author(s):  
Aqeel A Fatmi ◽  
Gregory V Williams ◽  
Elizabeth A Hickson

Abstract A reverse-phase liquid chromatographic method is described for the assay of medroxyprogesterone acetate in tablets. An octadecylsilane (C18) column with a mobile phase of methanol-O.OlM dibasic ammonium phosphate (80 + 20 v/v, pH 7.2 ± 0.1) and photometric detection at 254 nm separates medroxyprogesterone acetate from excipients. Detector responses were linear to concentrations of medroxyprogesterone acetate over the range 50-150 μg/mL (r = 0.999). Mean recovery of medroxyprogesterone acetate added to tablet excipients was 100.8%. Mean assay results were 101.3% (n = 3). The assay results are comparable to those obtained by the compendial liquid chromatographic method


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