首批立法保护岭南中药材中真菌毒素的LC-MS/MS法检测  

The First legislation to protect the detection of mycotoxins in Lingnan traditional Chinese medicine by LC-MS/MS

作　　者：胡佳哲 陈俏[1] 曹雅静 何嘉雯 赖宇红[1] 杨志业 HU Jia-zhe;CHEN Qiao;CAO Ya-jing;HE Jia-wen;LAI Yu-hong;YANG Zhi-ye(Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,广州510663

出　　处：《药物分析杂志》2020年第3期477-482,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：广东省中医药局“广东省首批立法保护中药材真菌污染状况研究与分析”(20172028);广东省科技厅粤港合作项目“岭南中药材质量标准及标准物质示范性研究”(2017A050506034)。

摘　　要：目的:建立了同时检测中药材中8种真菌毒素多残留的同位素标记-液相色谱-串联质谱分(LC-MS/RS)析方法。方法:采用LC-MS/MS法对首批立法保护的8种岭南中药材中真菌毒素污染分析。样品经甲醇-甲酸-水溶液(79∶1∶20)提取后,通过适当稀释和过滤,采用Thermo Hypersil GOLD色谱柱分离,0.1%甲酸乙腈-0.1%甲酸水为流动相,电喷雾正负离子扫描模式,同位素内标法定量。结果:结果表明在0.33~500μg·L-1范围,8种真菌毒素线性关系良好,r均大于0.999 0;检测下限为0.1~5.0μg·kg-1;平均回收率为80.3%~108.8%,RSD为0.10%~9.6%。共检测了108批中药材,检出率为16.7%,检出含量为1.0~99.4μg·kg-1。结论:LC-MS/MS法适用于中药材中多种真菌毒素的同时检测,首批立法保护中药材中存在着一定程度的真菌毒素残留,具有一定的健康风险,应当引起关注。Objective:To establish an isotope labeling-high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for simultaneous determination of multiple residues of eight mycotoxins in traditional Chinese medicines. Methods:The method was used to analyze the mycotoxin contamination in the first batch of eight Lingnan traditional Chinese medicines under legislative protection. Samples were extracted by methanol-formic acid-water(79∶1∶20),diluted and filtered properly. The separation of 8 mycotoxins was carried out a Thermo Hypersil GOLD chromatographic column,using 0.1% formic acid acetonitrile-0.1% formic acid solution,and determined in positive and negative electro-spray ionization mode. The isotope internal standards were employed for quantification. Results:Under the optimized conditions,the calibration curve showed good linearity in ranged from 0.33 μg·L-1 to 500 μg·L-1 with correlation coefficients greater than 0.999 0. The limits of detection(LODs)were 0.1-5.0 μg·kg-1. The recoveries of 8 mycotoxins at three levels were in the range of 80.3%-108.8%,the relative standand deviation(RSDs)were 0.10%-9.6%. 108 batches of Chinese herbal medicines were detected,the detection rate was 16.7%,the detection content was 1.0-99.4 μg·kg-1. Conclusion:This method is suitable for simultaneous detection of mycotoxins in traditional Chinese medicines. There are some mycotoxin residues in the first batch of legislation to protect traditional Chinese medicines,which have certain health risks and should arouse attention.

关 键 词：立法保护 中药材 真菌毒素 残留 污染 液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]