超高效液相色谱-质谱法同时检测中药酒剂中多种真菌毒素的污染水平  

Simultaneous Determinations of Multi-residue Mycotoxins in Chinese Medicine Health Wines by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李宁侠 唐招平 马宁[3] 

机构地区：[1]西安医学院第二附属医院检验科,陕西西安710038 [2]西北妇女儿童医院检验科,陕西西安710016 [3]宝鸡市中心医院病理科,陕西宝鸡721000

出　　处：《现代中药研究与实践》2017年第2期57-61,共5页Research and Practice on Chinese Medicines

摘　　要：目的基于多级反应监测模式-信息相关扫描方式-增强子离子扫描(MRM-IDA-EPI)辅助定性和定量方法,建立超高效液相色谱-电喷雾电离-串联质谱(UHPLC-ESI-MS/MS),同时测定中药酒剂中多种真菌毒素残留。方法样品采用QuEChERS方法进行前处理,UPLC-ESI-MS/MS法测定,流动相为0.1%甲酸-水(水相)和0.1%甲酸-甲醇(有机相),采用Acquity UPLC BEH C_(18)柱(150 mm×2.1 mm,I.D,1.7μm)进行分离,流速为0.3 ml/min,正/负离子模式监测。采用基质匹配标准曲线外标法定量分析。结果10种分析物在0.05~250 ng/ml浓度范围内线性关系良好,相关系数均大于0.999 2。定量限为0.04~0.60 ng/ml,加标回收率为79.9%~103.8%,相对标准偏差(RSD)小于5.1%。结论本研究前处理方法简单,检测方法准确、灵敏度高、检测速度快,已成功应用于各大超市随机购买的25批酒剂样品中多种真菌毒素残留的快速检测与确证。Objective To establish an ultra high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry （UHPLC-ESI-MS/MS） method based on multiple-reaction- monitoring information-dependent-acquisition enhanced-product-ion （MRM-IDA-EPI） which was used to determinate simultaneously multiple mycotoxins residues in Chinese medicine health wine. Methods The samples were treated by QuEChERS-based extraction procedure, determined by UFLC-ESI-MS/MS, separated on Acquity UPLC BEH C18 column （150 mm × 2.1 mm, I.D, 1.7 μm） with water-methanol （both containing 0.1% formic acid） system at the flow rate of 0.3 ml/min and monitored in positive/negative ion monitoring mode. Matrix-matched calibration curves with external standard method were used for accurate quantitation of target mycotoxins in real samples. Results Linearity was excellent in the concentration ranges of 0.05 - 250 ng/ml and correlation coefficients were more than 0.999 2. The limit of quantification was 0.04 - 0.60 ng/ml, and the mean recoveries were 79.9% - 103.8% with relative standard deviation （RSD） value was less than 5.1%. Conclusion In this study, the pretreatment method was simple and the method has high sensitivity and fast detection speed, which has been successfully applied to determine rapidly and confirm multiple mycotoxins residues in 25 batches of Chinese medicine health wine samples purchased in various supermarkets.

关 键 词：中药酒剂 真菌毒素 超高效液相色谱-串联质谱 QUECHERS 

分 类 号：R284[医药卫生—中药学]