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LC-MS/MS测定四大南药中黄曲霉毒素含量
引用本文:查玉兵,杨春亮,王晓芳,张珍,者永辉,林玲,曾绍东.LC-MS/MS测定四大南药中黄曲霉毒素含量[J].安徽农业科学,2014,42(36):12901-12903.
作者姓名:查玉兵  杨春亮  王晓芳  张珍  者永辉  林玲  曾绍东
作者单位:农业部食品质量监督检验测试中心(湛江),广东湛江524001;农业部农产品加工质量安全风险评估实验室(湛江),广东湛江524001;农业部食品质量监督检验测试中心(湛江),广东湛江,524001;西宁市动物卫生监督所,青海西宁,810000
基金项目:海南省自然科学基金,2014年农产品质量安全风险评估应急处置财政专项
摘    要:目的]采用高效液相色谱-串联质谱仪(LC-MS/MS),在多反应监测(MRM)模式下建立了四大南药中黄曲霉毒素(AFB1、AFB2、AFG1、AFG2)含量的测定方法.方法]试样中的黄曲霉毒素经甲醇/水(70/30)提取,黄曲霉毒素免疫亲和柱净化,液相色谱-串联质谱法测定,外标法定量.结果]该方法的检出限(LOD)为0.2~0.5 μg/kg,线性范围为0~50 μg/L,相关系数R2腰均大于0.999;在2~50μg/ks的添加水平上,4种霉菌毒素平均回收率为78.6% ~92.1%,相对标准偏差RSD为0.8% ~8.4%.结论]该方法前处理简单、快速,灵敏度、准确度和精密度高.

关 键 词:高效液相色谱-串联质谱  黄曲霉毒素  四大南药  含量

Determination of Aflatoxin contaminants in four south medicines by LC-MS/MS
Institution:ZHA Yu-bing;YANG Chun-liang;WANG Xiao-fang;Center for food quality supervision & testing ( Zhangjiang) Ministry of agriculture PRC;Labaratory of quality & safety risk assessment on agro-processing( Zhanjiang);
Abstract: Objective] The research aimed to develop the determination method of aflatoxin (AFB~ ,AFB2 ,AFG ,AFG2 )content in four southmedicines in the multiple reaction monitoring (MRM) mode by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Method ] The drugs were extracted with methanol/water( 70/30, V/V), and cleaned up by using beacon aflatoxin column, dissolved inmethanol and analysised by LC-MS/MS. Resuh~The limits of detection(LOD) were O. 2 -0.5 ixg/kg. The calibration curves were linear be-tween 0 to 50 txg/L, and the correlation coefficient was more than 0. 999. The average recoveries ranged from 78.6% - 92.1% and RSD was0.8% - 8.4% by addition of 2 - 50 p~g/kg avermectin standards to four south medicines as matrixes. Conclusion] The proposed method wasfast, simple, sensitive and accurate.
Keywords:UPLC-MS/MS  Aflatoxin  Four south medicines  Contaminants
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