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目的建立中药材中4种黄曲霉毒素测定的快速液相色谱-串联质谱方法。方法样品经体积分数70%甲醇提取、免疫亲和柱净化,岛津Shim-pack XR-ODS色谱柱,用甲醇-乙腈(1∶1)和水为流动相,梯度洗脱,ESI+扫描,多反应监测(MRM)。结果黄曲霉毒素B1在0.102 1~10.21 ng.mL-1内、黄曲霉毒素B2在0.061 2~7.65 ng.mL-1内、黄曲霉毒素G1在0.193~9.65 ng.mL-1内、黄曲霉毒素G2在0.121~7.55 ng.mL-1内,线性关系均良好,r>0.999 8;4种黄曲霉毒素回收率在77.0%~102.4%之间。结论本方法准确可靠,适合中药材中4种黄曲霉毒素含量的测定。
Objective To establish a rapid liquid chromatography - tandem mass spectrometry method for the determination of four aflatoxins in Chinese herbal medicines. Methods The samples were extracted with 70% methanol by volume fraction and purified by immunoaffinity column. Shimadzu Shim-pack XR-ODS column was eluted with methanol-acetonitrile (1: 1) Response Monitoring (MRM). Results Aflatoxin B1 was between 0.102 1 and 10.21 ng · mL-1, aflatoxin B2 was between 0.061 2 and 7.65 ng · mL-1, aflatoxin G1 was between 0.193 and 9.65 ng.mL-1, The linear range of toxin G2 was 0.121 ~ 7.55 ng.mL-1, r> 0.999 8. The recoveries of four aflatoxins ranged from 77.0% to 102.4%. Conclusion The method is accurate and reliable and suitable for the determination of four aflatoxins in traditional Chinese medicine.