摘要
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进行进一步的确证。结果:在优化条件下,黄曲霉毒素G2、G1、B2、B1分别在0.19~0.95,0.53~2.65,0.22~1.08,0.51~2.55 ng·mL^(-1)的范围内有良好的线性关系,r>0.999 5,回收率在86.2%~104.9%之间。结论:该方法操作简便,灵敏度高、重复性好、结果准确,可运用于安神益脑丸中黄曲霉毒素的检测。5批样品中有2批检出黄曲霉毒素,检出率为40%,建议增订该品种黄曲霉毒素的检查项。
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.
作者
谭静玲
丁晓萍
姜涛
费毅琴
黄丹丹
郑国华
TAN Jing-ling;DING Xiao-ping;JIANG Tao;FEI Yi-qing;HUANG Dan-dan;ZHENG Guo-hua(College of Pharmacy,Hubei University of Chinese Medicine,Hubei Wuhan 430065,China;Hubei Institute for Drug Control,Hubei Wuhan 430075,China;Hubei Engineering Research Center for Drug Quality Control,Hubei Wuhan 430075,China)
出处
《中国医院药学杂志》
CAS
北大核心
2021年第7期687-691,共5页
Chinese Journal of Hospital Pharmacy
基金
湖北省食品药品监督管理局科研项目(编号:201802005)。
