免疫亲和柱净化-液相色谱-串联质谱法测定中药材中的14种真菌毒素

依次采用磷酸盐缓冲液(PBS)和甲醇-PBS溶液提取样品,以多功能免疫亲和柱净化,采用液相色谱-串联四极杆质谱检测,可同时测定中药材中的黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、伏马毒素B1、伏马毒素B2、T-2毒素、HT-2毒素、赭曲霉毒素A(OTA)、玉米赤霉烯酮等14种真菌毒素。优化条件下,真菌毒素的定量限(LOQ)为1～5 μg/kg, 4种中药材基质(人参、桔梗、板蓝根、麦门冬)中3个不同添加水平的平均回收率(n=6)为71.9%～99.7%,相对标准偏差(RSD)为4.8%～15.8%。该方法的检测速度快,中药材复杂基质的干扰较少,结果准确、可靠,定量限可满足国内外中药材真菌毒素相关限量的要求。

Determination of 14 mycotoxins in Chinese herbs by liquid chromatography-tandem mass spectrometry with immunoaffinity purification

A method was developed for the determination of 14 mycotoxins,aflatoxins,T-2, HT-2,fumonisins,ochratoxin A,zearalenone,etc.in Chinese herbs by liquid chromatography-tandem quadrupole mass spectrometry(LC-MS/MS).The sample was extracted with phosphate buffer solution(PBS) and methanol in turn,and then purified by a high selective multifunctional immunoaffinity column.The column was washed by PBS(containing 0.1% Twain) and water,and then eluted by methanol.The eluate was dried under nitrogen,dissolved in meth...