分析化学2016，Vol.44Issue(6)：970-978,9.DOI:10.11895/j.issn.0253-3820.150229
复合免疫亲和柱净化-液相色谱-串联质谱法测定动物源食品中6种黄曲霉毒素和6种玉米赤霉醇类真菌毒素残留量
Determination of Aflatoxins and Zeranols in Animal-Originated Foods by High Performance Liquid Chromatography-Tandem Mass Spectrometry Combined With Immunoaffinity Clean-up Column
摘要
Abstract
A high performance liquid chromatography-tandem mass spectrometric ( HPLC-MS / MS) method coupled with an immunoaffinity clean-up column was successfully developed for determination of aflatoxins (AFB1 , AFB2 , AFG1 , AFG2 , AFM1 and AFM2 ) and zeranols ( α-zeranol, β-zeranol, α-zearalenol,β-zearalenol, zearalanone and zearalenone ). The sample was extracted with methanol-acetonitrile (20∶ 80, V/ V) after enzymatic digestion by β-glucuronidase / sulfatase, and the extraction solution was passed through glassy fiber filter paper and then diluted with phosphate buffer solution (PBS). The reconstituted solution was cleaned up with IAC-AZ immunoaffinity column, and then analyzed by HPLC-MS / MS in multiple reaction monitoring (MRM) mode. The results indicated that the linear detection range was 0. 03-6. 0 μg / L for AFB2 and AFG2 , and 0. 05-20 μg / L for the rest compounds. The correlation coefficients were above 0. 999. The limits of detection (LOD) and limits of quantitation (LOQ) were 0. 01-0. 03 μg / kg and 0. 04-0. 09 μg / kg, respectively. The recoveries of the aflatoxins and zeranols were in the range of 73. 6% -98. 4% at the spiked levels of 0. 5, 1 and 5 μg / kg, and the relative standard deviations (RSDs) were in the range of 1. 9% -11. 2% . The method was proved to be simple and accurate, and suitable for the rapid determination of aflatoxins and zeranols in animal-originated foods.关键词
动物源食品/复合免疫亲和柱/黄曲霉毒素/玉米赤霉醇类真菌毒素/高效液相色谱-串联质谱Key words
Animal-originated foods/Combination immunoaffinity column/Aflatoxins/Zeranols/High performance liquid chromatography-tandem mass spectrometry引用本文复制引用
孙雪,郗存显,唐柏彬,王国民,陈冬东,赵华..复合免疫亲和柱净化-液相色谱-串联质谱法测定动物源食品中6种黄曲霉毒素和6种玉米赤霉醇类真菌毒素残留量[J].分析化学,2016,44(6):970-978,9.基金项目
本文系科技部质检公益(No.201210086)项目和国家认监委检验检疫行业标准(No.2011B138)项目资助 （No.201210086）
