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Determination of Free Gossypol in Feed by Liquid Chromatography-Tandem Mass Spectrometry |
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DOI:10.3969/j.issn.1004-4957.年份.月份 |
KeyWord:feed gossypol liquid chromatography-tandem mass spectrometry(LC-MS/MS) |
Author | Institution |
ZHANG Wen-hua,XIE Wen*,CHEN Shu-bing,HUANG Cha-qun,SHEN Li |
1.浙江出入境检验检疫局;2.宁波出入境检验检疫局; 3.上海出入境检验检疫局 |
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Abstract: |
A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was developed for the determination of gossypol in feed.The sample was extracted with acetone-water(7∶3).The compound was separated on a C18 column(100 mm×2.1 mm,3.5 μm)with acetonitrile – 0.1% formic acid as mobile phase by gradient elution.The detection of gossypol was carried out by LC-MS/MS with positive electrospray ionization under the multiple reaction monitoring mode and quantified the external standard method.The limits of quantitation(S/N>10)was 1 mg/kg.Under the optimal conditions,the calibration curve was linear in the range of 10-100 μg/L with correlation coefficient of 0.993.The recoveries of gossypol at the spiked levels of 1,20,40 mg/kg in feed ranged from 83.8% to 97.5% with relative standard deviations(RSDs)of 1.3%-5.2%.With the advantages of easy operation,higher recoveries and good precision,the method was suitable for the confirmation and quantification of gossypol residue in feed. |
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