安神益脑丸中黄曲霉毒素残留量测定及LC-QQQ/MS确证

目的:建立高效液相色谱-荧光检测器测定安神益脑丸中黄曲霉毒素G2、G1、B2、B1的方法;分析安神益脑丸中黄曲霉毒素的污染情况.方法:待测样品采用80％乙腈作为提取溶剂,经免疫亲和柱净化、高效液相色谱分离、光化学柱后衍生后,通过荧光检测器测定其中黄曲霉毒素的含量;采用超高效液相色谱串联三重四极杆质谱法对以上实验测定结果...

Determination of aflatoxin residuesin Anshen Yinao pills and LC-QQQ/MS

OBJECTIVE To establish an HPLC with fluorescent detector (HPLC-FLD) method for determining aflatoxin (AF) G₂, G₁, B₂ and B₁ in Anshen Yinao pills and explore the safety of the preparation.METHODS After extraction with 80% acetonitrile and purification by immunoaffinity columns, AF G₂, G₁, B₂ and B₁ in samples were analyzed by HPLC-FLD with post-column photochemical derivatization. The results from HPLC-FLD analysis were further confirmed by rapid resolution liquid chromatography coupled to triple quadruple mass spectrometry (UPLC-QQQ/MS).RESULTS Under optimal conditions, AFG₂, G₁, B₂ and B₁ showed excellent linear relationships at the ranges of 0.19-0.95, 0.53-2.65, 0.22-1.08 and 0.51-2.55 ng·mL^-1 respectively (r>0.999 6). The recoveries of aflatoxin G₂, G₁, B₂ and B₁ were 86.2%-104.9%.CONCLUSION The above method has demonstrated convenient operation, good repeatability, high sensitivity and accuracy. The positive detection rate of 5 batches for aflatoxin was 40% (2 batches). It is advisable to add the determination of AFs into the quality control of Anshen Yinao pills.