超高效液相色谱串联质谱法检测三七药材中10种真菌毒素  

Determination of 10 mycotoxin contaminants in Panax notoginseng by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：陈勇[1] 陈重均[1] 李劲[1] 栾连军[1] 刘雪松[1] 吴永江[1] 

机构地区：[1]浙江大学药学院,浙江杭州310058

出　　处：《药学学报》2015年第1期81-85,共5页Acta Pharmaceutica Sinica

基　　金：教育部博士点基金资助项目(20110101110121)

摘　　要：为保证中药三七质量和安全性,本文建立了一种同时检测三七药材中10种真菌毒素的超高效液相色谱串联质谱定量分析方法。三七药材以乙腈超声提取,多功能净化柱（HLB柱）净化,Phenomenex Kinetex XB-C18柱分离,用甲醇和含5 mmol·L^-1醋酸铵水溶液为流动相进行梯度洗脱,以电喷雾离子源正负离子模式多反应监测方式检测。结果表明,10种毒素在各自线性范围内线性关系良好,相关系数r在0.998 1~1.000 0之间,定量限为0.15~8.6μg·kg^-1,加标回收率为73.8%~107.0%,相对标准偏差为0.10%~10.9%。该方法净化效果好、灵敏度高、重复性好,适用于基质成分复杂的三七药材中多种真菌毒素的定量检测。To ensure the quality and safety of Panax notoginseng, a method for the simultaneous determination of 10 mycotoxins in Panax notoginseng was developed using ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. The sample was extracted with acetonitrile and purified by HLB multifunction cleanup column. The separation was performed on a Phenomenex Kinetex XB-C18 column by gradient elution using methanol and 5 mmol.L^-1 ammonium acetate as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization （ESI） source operated in both positive and negative ionization modes. The linear relationships of the 10 mycotoxins were good in their respective linear ranges. The correlation coefficients （r） ranged from 0.998 1 to 1.000 0. The LOQs of the 10 mycotoxins were between 0.15 and 8.6μg·kg^-1. The average recoveries ranged from 73.8% to 107.0% with relative standard deviations （RSDs） of 0.10%-10.9%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in Panax notoginseng.

关 键 词：真菌毒素 超高效液相色谱串联质谱 三七 

分 类 号：R917[医药卫生—药物分析学]