SPE-HPLC-MS/MS测定祛痘类化妆品中8种非法添加药物

    Determination of 8 Illegal Added Drugs in Anti-acne Cosmetics by SPE-HPLC-MS/MS

    • 摘要:
      目的 采用固相萃取-高效液相色谱串联质谱法(SPE-HPLC-MS/MS)建立同时测定3种不同基质类型(水剂类、乳液类和膏霜类)祛痘化妆品中氟康唑、酮康唑、硝酸益康唑、硝酸咪康唑、盐酸萘替芬、他扎罗汀、依曲替酯和维胺酯8种非法添加药物的检测方法。
      方法 化妆品样品经含有1%四氢呋喃的甲醇溶液提取后,采用HLB固相萃取柱净化后上机检测,经ZORBAX-C18柱分离,0.1%甲酸水溶液-含0.1%甲酸的甲醇溶液作为流动相梯度洗脱,在电喷雾离子源正离子模式下电离,多反应监测模式下测定,基质匹配标准曲线法定量。
      结果 8种化合物在各自浓度范围内线性关系良好,相关系数均≥0.995,检出限为0.015~0.16 mg·kg−1,定量限为0.045~0.48 mg·kg−1,平均回收率为89.5%~103.1%,RSD均<10%。
      结论 本法简便、准确、灵敏度高,可用于祛痘类化妆品中8种非法添加药物的检测。

       

      Abstract:
      OBJECTIVE To establish a solid phase extraction-high performance liquid chromatography tandem mass spectrometry(SPE-HPLC-MS/MS) method for the simultaneous determination of 8 illegal added drugs(i.e., fluconazole, ketoconazole, econazole nitrate, miconazole nitrate, naftifine hydrochloride, tazarotene, etretinate and viaminate) in anti-acne cosmetics with 3 different matrix types(water-based, lotion and cream).
      METHODS Cosmetic samples were extracted by methanol solution containing 1% tetrahydrofuran, and purified by HLB prior to injection. The separation was performed on a ZORBAX-C18 column with gradient elution using 0.1% formic acid aqueous solution and methanol solution containing 0.1% formic acid as the mobile phase. The ionization was carried out in positive ion mode using an electrospray ionization source, and the determination was performed in multiple reaction monitoring mode. The quantification was achieved by the matrix-matched calibration curve method.
      RESULTS Eight compounds had good linear relationship in their respective concentration range, the correlation coefficient was ≥0.995, the detection limit was 0.015−0.16 mg·kg−1, the quantitative limit was 0.045−0.48 mg·kg−1, and the average recovery was 89.5%−103.1%, the RSD was <10%.
      CONCLUSION The method is simple, accurate and sensitive, which can be used for the detection of 8 illegal added drugs in anti-acne cosmetics.

       

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