红药片中黄曲霉毒素的含量测定及限度研究  

Determination and limit of aflatoxins in Hongyao tablets

作　　者：张耀文 李尚颖 隋晓璠 徐万魁 ZHANG Yao-wen;LI Shang-ying;SUI Xiao-fan;XU Wan-kui(Liaoning Inspection,Examination&Certification Centre,Liaoning Institute for Drug Control,State Key Laboratory of Chemical Drug Quality Research and Evaluation,Shenyang 110036)

机构地区：[1]辽宁省检验检测认证中心,辽宁省药品检验检测院,化学药品质量研究与评价国家重点实验室,沈阳110036

出　　处：《中南药学》2024年第8期2177-2181,共5页Central South Pharmacy

基　　金：辽宁省自然科学基金(No.2020-MS-073)。

摘　　要：目的建立高效液相色谱-质谱联用法测定红药片中黄曲霉毒素(以黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1和黄曲霉毒素G2总量计)的含量,制订红药片中黄曲霉毒素的限度。方法以Venusil MP C18(4.6 mm×150 mm,5μm)为色谱柱;流动相为2 mmol·L^(-1)醋酸铵溶液(A)-甲醇(B),梯度洗脱;串联质谱仪检查,电喷雾离子源(ESI),正离子检测模式。结果黄曲霉毒素B1在0.0108~54.0 ng·mL^(-1)、黄曲霉毒素B2在0.0145~14.5 ng·mL^(-1)、黄曲霉毒素G1在0.0101~50.5 ng·mL^(-1)、黄曲霉毒素G2在0.0150~15.0 ng·mL^(-1)内与峰面积线性关系良好。黄曲霉毒素B1、B2、G1和G2回收率分别为89.24%、80.31%、87.06%和74.19%(n=6);重复性RSD分别为2.9%、4.6%、3.3%和5.0%。6批红药片中的黄曲霉毒素B1、B2、G1和G2的含量及总量均小于所制订的黄曲霉毒素限度,结果均符合规定。结论本试验建立了高效液相色谱-质谱联用法测定红药片中黄曲霉毒素的含量,并制订了红药片中黄曲霉毒素的限度,为其他中成药的黄曲霉毒素含量的检测及限度的制订提供了新的思路和理论参考。Objective To establish a liquid chromatography-mass spectrometry(HPLC-MS)method for the determination of aflatoxins(aflatoxins B1,aflatoxins B2,aflatoxins G1 and aflatoxins G2)in Hongyao tablets,and to set limits on the amount of aflatoxins in Hongyao tablets.Methods The chromatographic column was Venusil MP C18(4.6 mm×150 mm,5μm).The mobile phase consisted of 2 mmol·L^(-1)ammonium acetate solution(A)-methanol(B)with gradient mode.Electrospray ionization source(ESI)was used for the determination by tandem mass spectrometer,and the positive ion mode was adopted.Results The linear calibration curves were obtained at 0.0108~54.0 ng·mL^(-1)for aflatoxins B1,0.0145~14.5 ng·mL^(-1)for aflatoxins B2,0.0101~50.5 ng·mL^(-1)for aflatoxins G1,and 0.0150~15.0 ng·mL^(-1)for aflatoxins G2,respectively.The recoveries of aflatoxins B1,B2,G1 and G2 were 89.24%,80.31%,87.06%and 74.19%,respectively.The RSDs of repeatability were 2.9%,4.6%,3.3%and 5.0%,respectively.The content and total amount of aflatoxins B1,B2,G1 and G2 in 6 batches of Hongyao tablets were all lower than the aflatoxins limits.Conclusion The HPLC-MS method is established for the determination of aflatoxins in Hongyao tablets,and the limit of aflatoxins in Hongyao tablets is established at the same time,which provids a new idea and theoretical reference for the determination of aflatoxins content in other proprietary Chinese medicines.

关 键 词：红药片 黄曲霉毒素 高效液相色谱-质谱联用法 TD50 

分 类 号：R927[医药卫生—药学]