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采用超高效液相色谱建立了化妆品中苔黑醛和氯化苔黑醛的分析方法,并采用液相色谱-串联质谱法进行确证。化妆品试样采用5%三氯乙酸-乙腈混合溶液(70/30,V/V)超声提取15 min,离心过膜后即可直接上机分析。采用亚二微米超高效液相色谱柱分离,外标法定量;质谱确证采用水和乙腈作为流动相梯度洗脱,电喷雾负离子模式电离,多反应监测模式检测。苔黑醛和氯化苔黑醛在0.1~50 mg/L范围内线性关系良好(线性相关系数r≥0.9990),方法的定量限为5.0 mg/kg(信噪比为10)。膏霜、乳液和香水等样品在5.0,10,25 mg/kg的添加回收率在87.4%~96.3%之间,RSD(n=6)为1.4%~4.6%。方法适用于化妆品中苔黑醛和氯化苔黑醛的检测及其含量水平的普查。
The method for the determination of mepigenol and chlorhexidine aldehyde in cosmetics was established by ultra performance liquid chromatography and confirmed by liquid chromatography-tandem mass spectrometry. Cosmetic samples were extracted with 5% trichloroacetic acid-acetonitrile mixed solution (70/30, V / V) for 15 min and centrifuged directly to the machine for analysis. Sub-two-micron ultra-high performance liquid chromatography column separation, external standard quantitative; mass spectrometry confirmed the use of water and acetonitrile gradient elution, electrospray negative ion mode ionization, multi-reaction monitoring mode detection. There was a good linear relationship between mossyphenol and meclofenoxate in the range of 0.1-50 mg / L (linear correlation coefficient r ≥ 0.9990). The limit of quantification for this method was 5.0 mg / kg (signal to noise ratio 10). The recoveries of samples with creams, lotions and perfumes ranged from 87.4% to 96.3% at 5.0, 10 and 25 mg / kg with RSD (n = 6) from 1.4% to 4.6%. The method is suitable for the determination and determination of the content of capsaic aldehyde and chlorhexidine aldehyde in cosmetics.