High-Speed Liquid Chromatographic Determination of Monensin, Narasin, and Salinomycin in Feeds, Using Post-Column Derivatization

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%.

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.


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%.


1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.


1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger

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.


1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


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.


1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.


1975 ◽  
Vol 58 (5) ◽  
pp. 1013-1014
Author(s):  
Samuel K Reeder

Abstract A simple, direct, and rapid method is given for the analysis of citrus oils for the fungistat biphenyl by high-speed liquid chromatography. The method is extended to orange juice and various “dry flavors” by an extraction procedure. Analytical limits are <1 ppm without need for any cleanup or concentration steps.


1971 ◽  
Vol 54 (3) ◽  
pp. 551-554 ◽  
Author(s):  
N E Skelly ◽  
R F Cornier

Abstract A semiautomated ion exchange-ultraviolet procedure has been developed for the determination of clopidol in poultry feed at the 40–250 ppm level. A methanol extract of the feed is injected into an alumina precolumn to remove interferences. The clopidol passes through the alumina column and is collected on an ion exchange column. With a specially designed elution apparatus the clopidol is removed by an acetic acid-methanol gradient. The eluate proceeds through a flowcell mounted in an ultraviolet spectrophotometer. Response of the spectrophotometer is monitored by a recorder. Concentration is determined by comparing the peak area in the resulting chromatogram with that of a standard. Accuracy and precision of this method are ±5% relative to the amount present (100±5 ppm).


1995 ◽  
Vol 78 (5) ◽  
pp. 1177-1182 ◽  
Author(s):  
Victor S Sobolev ◽  
Richard J Cole ◽  
Joe W Dorner ◽  
Boris Yagen

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.


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