超高效液相色谱-离子淌度飞行时间质谱法测定辅料中22种真菌毒素  

Determination of 22 mycotoxins in pharmaceutical excipients by UHPLC-IM TOF MS

作　　者：胡佳哲 刘亚雄[1] 赖宇红[1] 叶秀金[1] 王淼[1] 杨志业 HU Jia-zhe;LIU Ya-xiong;LAI Yu-hong;YE Xiu-jin;WANG Miao;YANG Zhi-ye(Guangdong Institute for Drug Control,Key Laboratory of Quality Control and Evaluation of Pharmaceutical Excipients,SFDA,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,国家药监局药用辅料质量控制与评价重点实验室,广州510663

出　　处：《药物分析杂志》2024年第3期434-441,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：广东省药品监督管理局科技创新项目(2023TDZ04);广东省药品检验所科研项目(ZA20200025)。

摘　　要：目的:建立超高效液相色谱-离子淌度飞行时间质谱法同时检测药用辅料中22种真菌毒素的分析方法。方法:采用Waters CORTECS^(■)UPLC^(■)C_(18)(100 mm×2.1 mm,1.6μm)色谱柱,以0.1%甲酸水溶液-乙腈甲醇混合溶液(60∶40)为流动相,梯度洗脱,流速0.25 mL·min^(-1),柱温35℃。采用电喷雾离子源,MSe数据采集模式,正、负离子扫描模式,外标法定量。结果:22种真菌毒素在质量浓度为0.2~500μg·L^(-1)范围内,线性关系良好(r均大于0.9985);检测限为0.1~2.0μg·kg^(-1);平均回收率为80.4%~118.2%,RSD为0.20%~8.8%;22种真菌毒素的基质效应不明显。应用该方法检测了32批次玉米淀粉和167批次糊精,其中一些批次检出黄曲霉毒素B1、伏马毒素B1、伏马毒素B2和玉米赤霉烯酮。结论:该方法准确、高效和稳定,可为药用辅料中真菌毒素风险评估提供方法参考。Objective:To establish a method for the determination of 22 mycotoxins in pharmaceutical excipients by ultra-high performance liquid chromatography-ion mobility time-of-flight mass spectrometry(UHPLC-IM TOF MS).Methods:The samples were separated on a Waters CORTECS^(■)UPLC^(■)C_(18)(100 mm×2.1 mm,1.6μm)column by gradient elution at a flow rate of 0.25 mL·min^(-1)using 0.1%formic acid and a mixture of acetonitrile and methanol(60∶40)as the mobile phase.The column temperature was maintained at 35℃.MSe data acquisition mode was chosen and electrospray ion source operating in the positive/negative ionization mode for data acquisition was applied.The external standard method was used for quantification.Results:22 mycotoxins showed good linear relationships within their respective ranges(r>0.9985).The limits of detection were 0.1-2.0μg·kg^(-1).The recoveries of 22 mycotoxins at three levels were in the range of 80.4%-118.2%,and the RSDs were 0.20%-8.8%.The matrix effect of 22 mycotoxins was not obvious.The method was applied to the detection of 32 batches of corn starch and 167 batches of dextrin.Aflatoxin B1,fumonisins B1 and B2,and zearalenone were detected in some batches.Conclusion:The method is accurate,efficient and stable.It can be used in quality control of mycotoxins in pharmaceutical excipients,and provides technical supports for the risk assessment of mycotoxins.

关 键 词：药用辅料 真菌毒素 糊精 玉米淀粉 玉米赤霉烯酮 伏马毒素 黄曲霉毒素 超高效液相色谱-离子淌度飞行时间质谱 有毒有害污染物 

分 类 号：R917[医药卫生—药物分析学]