超高效液相色谱-串联质谱法快速测定洗发育发类化妆品中6种违禁药物

Rapid Screening and Quantitative Detection of 6 Prohibited Drugs in Shampoo and Hair Growth Cosmetics by UPLC-MS/MS

  • 摘要: 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法同时检测洗发育发类化妆品中6种违禁药物。样品经甲醇超声萃取,用 Waters Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm×1.7 μm)分离,以甲醇和0.1%甲酸-水溶液为流动相梯度洗脱,在电喷雾正离子模式下,采用多反应监测(MRM)模式进行定性和定量分析。结果表明,6种药物在各自线性范围内的线性关系良好,相关系数(R2)均大于0.997,检出限为0.9~13.3 μg/kg,3个加标水平下的回收率在84.0%~94.7%之间,RSD在1.3%~5.6%(n=6)之间。该方法准确、简便,可用于洗发育发类化妆品中违禁药物的快速检测。

     

    Abstract: Baldness, alopecia and acne are common skin and hair diseases that may adversely influence the patient’s social relationships. For reasons of safety and ease of use, cosmetic products are widely used to control these diseases. However, for the sake of profit and to enhance short-term efficacy, some manufacturers illegally add synthetic drugs to their cosmetic products. According to previous reports, minoxidil, flutamide, spironolactone, finasteride, dutasteride and ketoconazole are the most common topically active anti-alopecia, anti-baldness, and anti-acne drugs. Electrospray ionisation mass spectrometry (ESI-MS) is suitable for detecting these substances in an illegal product at lower concentrations, with a high degree of specificity, and obtaining additional information about the structure of the analytes. In this study, a method of ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for rapid screening and quantification of six prohibited drugs in shampoo and hair growth cosmetics. The sample was ultrasonic extracted with methanol and separated on Waters Acquity UPLC BEH C18 column(100 mm×2.1 mm×1.7 μm). The electrospray ionization source in positive ion mode was used for analysising the six prohibited drugs in the multiple reaction monitoring (MRM) mode. The results indicated that the standard curves were obtained with good correlation coefficients (R2>0.997) in their concentration ranges. The limits of quantitation for six benzotriazole ultraviolet stabilizers were in the range of 0.9-13.3 μg/kg. The mean recoveries at three spiked levels were 84.0%-94.7% with the relative standard deviations of 1.3%-5.6%. Twenty kinds of shampoo and hair growth cosmetics were tested, where no prohibited drugs was found. This method is accurate, simple, rapid, which is suitable for rapid screening and detection of prohibited drugs in shampoo and hair growth cosmetics.

     

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