液质联用法测定祛痘化妆品中125种禁用药物成分

DOI:Simultaneous Determination of 125 Prohibited Drugs in Anti-acne Cosmetics by HPLC-MS/MS

关键词:  HPLC-MS/MS法  祛痘化妆品  禁用药物

Key words:  HPLC-MS/MS  anti-acne cosmetics  prohibited drugs

摘要:

目的 建立一种高效液相色谱-串联质谱测定祛痘化妆品中125种禁用药物成分(激素类62种、抗感染类51种、维甲酸类8种、其他类4种)的方法。方法 样品用80%甲醇溶液为溶剂,超声提取后过滤膜上机分析,以XBridge UPLC? BEH C18色谱柱分离,5 mmol.L-1的乙酸铵溶液(含0.05%甲酸)-甲醇为流动相梯度洗脱,电喷雾正/负离子模式下,采用自动分段多反应检测模式采集数据,基质外标法进行定量。结果 125种禁用药物成分在各自的质量浓度范围内均呈良好的线性关系,相关系数均＞0.995。在4个不同浓度添加水平下,平均加标回收率为73 %~133 %,重复性相对标准偏差RSD(n=6)≤12 %。结论 该方法具有前处理简单、灵敏度高、专属性强、定性定量一次完成、分析时间短等特点,适用于祛痘类化妆品中125种禁用药物成分的检测。

Abstract:

ABSTRACT: OBJECTIVE To establish a HPLC-MS/MS method for simultaneous determination of 125 prohibited drugs in anti-acne cosmetics. METHODS The sample was dispersed with 80% methol solution for ultrasonic extraction. The separation and analysis was performed on a XBridge UPLC? BEH C18 column. The mobile phase consisted of methol - 5mmol/L ammonium acetate aqueous solution（within 0.05% formic acid）by gradient elution. Electrospray ionization source was applied and operated in the positive mode and negative mode(ESI+/ESI-). Schdule multiple reaction monitoring(sMRM) mode was used to monitor ions. Matrix-matched calibration was used to quantitative calculation. RESULTS 125 prohibited drugs showed good linear relationship in their ranges, the linear correlation coefficients of the method were >0.995. At four levels, the average recoveries ranged from 73% to 133%, with the RSD(n=6) not more than 12%. CONCLUSION The method is simple, rapid, selective, sensitive and accurate, and can be used for the determination of 125 prohibited drugs in anti-acne cosmetics.