液质联用法测定祛痘化妆品中125种禁用药物成分

贾艾玲; 陈春晓; 陈惠玲

doi:10.13748/j.cnki.issn1007-7693.20242942

液质联用法测定祛痘化妆品中125种禁用药物成分

Simultaneous Determination of 125 Prohibited Drugs in Anti-acne Cosmetics by LC-MS/MS

摘要

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，甲醇-5 mmol·L⁻¹的乙酸铵溶液(含0.05%甲酸)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:
OBJECTIVE To establish an LC-MS/MS method for simultaneous determination of 125 prohibited drugs(62 hormones, 51 anti infectives, 8 retinoids and 4 others) in anti-acne cosmetics.
METHODS The sample was dispersed with 80% methanol solution for ultrasonic extraction. The separation and analysis were performed on an XBridge UPLC^® BEH C₁₈ column. The mobile phase consisted of methanol-5 mmol·L⁻¹ 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⁻). Schedule multiple reaction monitoring(sMRM) mode was used to monitor ions. Matrix-matched calibrations were used to quantitative calculation.
RESULTS The 125 prohibited drugs showed good linear relationship in their respective mass concentration ranges, and the correlation coefficients were all > 0.995. At four different concentration levels, the average recoveries were 73%–133%, and the relative standard deviation(RSD)(n=6) were not more than 12%.
CONCLUSION This method has the characteristics of simple pretreatment, high sensitivity, strong specificity, one-time qualitative and quantitative analysis, and short analysis time. It is suitable for the determination of 125 prohibited drugs in anti-acne cosmetics.

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