UPLC-MS/MS检测浙产延胡索中4种黄曲霉毒素

Determination of Four Kinds of Aflatoxin in Zhejiang Corydalis Rhizoma by UPLC-MS/MS

目的建立延胡索中黄曲霉毒素(aflatoxin,AF)超高效液相色谱-三重四级杆质谱检测方法。方法以Agilent Zorbax Eclipse C18(2.1 mm×50 mm,1.8μm)色谱柱分离,在电喷雾离子源(ESI)正离子模式下电离,多反应监测(MRM)模式下测定。结果样品用70%甲醇提取,检测20批延胡索中的AFB1、AFB2、AFG1、AFG2。4种AF质谱检测的线性范围宽,相关性好,r≥0.997;回收率78.3%~93.7%;重复性RSD为1.5%~2.7%(n=6)。结论该方法专属性强,灵敏度高,重复性好,适用于延胡索中AF的检测,鉴于市场上延胡索饮片的AF风险较高,建议中国药典增加延胡索的AF检测。

OBJECTIVE To establish a method for the determination of aflatoxin(AF)in Corydalis Rhizoma by UPLC-MS/MS.METHODS Agilent Zorbax Eclipse C18(2.1 mm×50 mm,1.8μm)column was used for separation.Detection was carried out by positive electrospray ionization(ESI)mass spectrometer in multiple reaction monitor(MRM)mode.RESULTS Twenty samples were extracted with 70%methanol solution and AFB1,AFB2,AFG1 and AFG2 were detected.All the 4 kinds of aflatoxin compounds showed good linearity in their reasonable ranges,r≥0.997.The average recoveries of all the compounds were in range of 78.3%-93.7%,the RSD were 1.5%-2.7%(n=6).CONCLUSION The method is specific,sensitive and reproducible which is suitable for the detection of AF in Corydalis Rhizoma.In view of the risk of AF which exists in the market of Corydalis Rhizoma,suggested the addition of the quality examination method in Chinese Pharmacopoeia.