郑润生;徐晖;王文丽;詹若挺;陈蔚文;
ZHENG Run-sheng;XU Hui;WANG Wen-li;ZHAN Ruo-ting;CHEN Wei-wen;Research Center of Chinese Herbal Resource Science and Engineering,Key Laboratory of Chinese Medicinal Resource from Lingnan,Ministry of Education,Guangzhou University of Chinese Medicine;

• 1:广州中医药大学中药资源科学与工程研究中心 岭南中药资源教育部重点实验室

摘要(Abstract)：

基质效应是影响液质联用定量准确性的一个重要因素,在方法学评价阶段中必不可少。该研究采用稀释法,并通过优化色谱和质谱条件,成功克服苦杏仁的基质效应对整个分析过程的干扰,建立了一种可对苦杏仁污染黄曲霉毒素B1,B2,G1,G2进行大量筛查及检测的液质联用方法,与Mycosep226净化柱纯化的方法相比,具有回收率高、经济、简便的特点;对11批样品进行检测发现有2批样品的黄曲霉毒素检测结果呈阳性,其中黄曲霉毒素B1的污染水平为1.590².340μg·kg-1,黄曲霉毒素总量(B1+B2+G1+G2)的污染水平为2.3402.340μg·kg-1,黄曲霉毒素总量(B1+B2+G1+G2)的污染水平为2.340³.304μg·kg-1,表明苦杏仁污染黄曲霉毒素这一现象应当引起重视,并且有必要对其贮藏方式进行考察,以减少黄曲霉毒素的污染。
A simple,rapid and cost-effective high-performance liquid chromatography-tandem mass spectrometry( LC-MS/ MS) method was established for simultaneous determination of aflatoxins( AFB 1,AFB 2,AFG 1,AFG 2) in Armeniacae Semen Amarum and the application was performance in 11 samples collected from different markets,medical stores and hospitals. The sample was extracted with 84% acetonitrile/water and 250 μL extraction was directly injected into a LC-MS/MS system without further purification procedure after being redissolved with methanol. The LC separation was performed on a C 18 column with a linear gradient elution program of 4 mmol·L- 1NH 4 Ac-0. 1% formic acid solution and menthol as the mobile phase. Selected reaction monitoring( SRM) was used for selective determination of the four aflatoxins on a triple quadruple mass spectrometer,which was operated in positive ionization modes. All the four aflatoxins showed a good linear relationship with r > 0. 999 0,the average recoveries were between 87. 88% and 102. 9% and the matrix effect was ranged from 90. 71% to 99. 30% in low,intermediate and high levels. Furthermore,the higher recovery was obtained by the method reported in this study,comparing to the cleanup procedure with the Mycosep 226 purification column. Eleven samples collected were detected and the contamination levels of the AFB 1 were between 1. 590-2. 340 μg·kg- 1and the AF( B 1 + B 2 + G 1 + G 2) was ranged from 2. 340 to 3. 340 μg·kg- 1. In summary,the developed method was suitable to detect and screen AFB 1,AFB 2,AFG 1,AFG 2 in Armeniacae Semen Amarum.

关键词(KeyWords)： 液质联用技术;中药饮片;苦杏仁;黄曲霉毒素;真菌毒素
LC-MS/MS;Chinese crude drugs;Armeniacae Semen Amarum;aflatoxins;mycotoxins

Abstract:

Keywords:

基金项目(Foundation): 中央财政支持地方高校发展专项资金项目(粤财教[2010]358号)

作者(Authors): 郑润生;徐晖;王文丽;詹若挺;陈蔚文;
ZHENG Run-sheng;XU Hui;WANG Wen-li;ZHAN Ruo-ting;CHEN Wei-wen;Research Center of Chinese Herbal Resource Science and Engineering,Key Laboratory of Chinese Medicinal Resource from Lingnan,Ministry of Education,Guangzhou University of Chinese Medicine;

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