液质联用法同时测定多种基质祛痘化妆品中8种维甲酸类药物

    Simultaneous Determination of 8 Retinoid Drugs in Manifold Matrixes of Anti-acne Cosmetics by LC-MS/MS

    • 摘要:
      目的  建立高效液相色谱-串联质谱法同时测定多种基质祛痘化妆品中8种维甲酸类药物(他卡西醇、他扎罗汀、阿维A、异维甲酸、维甲酸、依曲替酯、维胺酯、阿达帕林)的方法。
      方法  样品加入1 mL饱和氯化钠溶液分散,用甲醇为溶剂,超声提取后过滤膜上机分析,以ACQUITY UPLC® BEH C18色谱柱(2.1 mm×100 mm,1.7 μm)分离,甲醇(含0.1%甲酸)-5 mmol·L−1的乙酸铵溶液(用冰醋酸调节pH值至4.0)为流动相梯度洗脱,电喷雾正/负离子模式下,自动分段多反应监测扫描,基质外标法进行定量。
      结果  8种维甲酸类药物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>0.996。在3个不同浓度添加水平下,平均加标回收率为75%~120%,相对标准偏差RSD(n=6)<10%。方法检出限除他卡西醇为0.4 mg·kg−1外,其余7种组分均为0.02 mg·kg−1
      结论  该方法具有前处理简单、专属性强、灵敏度高、准确性好、分析时间短等特点,适用于祛痘类化妆品中8种维甲酸类药物成分的检测。

       

      Abstract:
      OBJECTIVE  To establish an LC-MS/MS method for simultaneous determination of 8 retinoid drugs including tacalcitol, tazarotene, acitretin, isotretinoin, tretinoin, etretinate, viaminate, adapalene in manifold matrixes of anti-acne cosmetics.
      METHODS  The sample was dispersed with 1 mL saturated sodium chloride solution and then added methol solvent for ultrasonic extraction. The separation and analysis was performed on an ACQUITY UPLC® BEH C18 column((2.1 mm×100 mm, 1.7 μm). The mobile phase consisted of methanol containing 0.1% formic acid-5 mmol·L−1 ammonium acetate aqueous solution(adjust pH to 4.0 with acetic acid) by gradient elution. Electro-spray ionization 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 calibration was used to quantitative calculation.
      RESULTS  Eight retinoid drugs showed good linear relationship in their ranges, the linear correlation coefficients of the method were >0.996. At three different levels of addition, the average recoveries ranged from 75% to 120%, with the RSD(n=6) not more than 10%. The method detected concentration were 0.02 mg·kg−1 except for 0.4 mg·kg−1 of tacalcitol.
      CONCLUSION  The method is simple, selective, sensitive, accurate and rapid with short analysis time, and can be used for the determination of 8 retinoid drugs in anti-acne cosmetics.

       

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