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    QuEChERS结合超高压液相色谱-三重四极杆串联质谱法测定化妆品中5种禁用组分的含量

    Determination of 5 Prohibited Components in Cosmetics by Ultra-High Pressure Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry Combined with QuEChERS

    • 摘要: 提出了同时测定不同基质化妆品中环磷酰胺、氮杂环己醇、胃安、那可丁和美替拉酮等5种禁用组分含量的题示方法。水乳类和精油类化妆品样品经甲醇提取,霜膏类化妆品样品经饱和氯化钠溶液分散,无水乙醇提取,然后均采用十八烷基硅烷键合硅胶(C18)净化,以Waters BEH C18色谱柱分离,以不同体积比的0.1%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱,电喷雾离子源正离子模式下进行多反应监测(MRM)模式质谱分析,基质匹配法定量。结果显示,5种禁用组分的质量浓度在5~200 μg·L−1内与对应的峰面积呈线性关系,检出限(3S/N)为5~100 μg·kg−1。在不同空白基质中进行3个浓度水平的加标回收试验,5种禁用组分的回收率为90.1%~115%,测定值的相对标准偏差(n=6)为2.0%~14%。

       

      Abstract: The method mentioned by the title was proposed for simultaneous determination of 5 prohibited components including cyclophosphamide, azacyclonol, aminopentamide, narcotine and metyrapene in different cosmetic matrices. The samples of water emulsion and essential oil cosmetics were extracted with methanol, and the samples of cream cosmetics were dispersed with saturated sodium chloride solution and extracted with anhydrous ethanol. Then both were purified with octadecyl silane boned silica gel (C18). The targets were separated on Waters BEH C18 column using a mixed solution of 0.1% (volume fraction) formic acid solution and acetonitrile at different volume ratios as the mobile phase for gradient elution. Multiple reaction monitoring (MRM) mode in mass spectrometry analysis was carried out under positive ion mode of electrospray ion source, and matrix matching method was used for quantitative analysis. As shown by the results, linear relationships between the corresponding peak areas and mass concentrations of 5 prohibited components were found in the range of 5-200 μg·L−1, with detection limits (3S/N) in the range of 5-100 μg·kg−1. Test for recovery at 3 concentration levels was conducted in different blank matrices, and the recoveries of 5 prohibited components ranged from 90.1% to 115%, with RSDs (n=6) of the determined values in the range of 2.0%-14%.

       

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