化妆品中4种美白功效成分的高效液相色谱-串联质谱测定法

目的建立化妆品中4种美白功效成分(4-甲氧基水杨酸钾、苯乙基间苯二酚、二甲氧基甲苯基-4-丙基间苯二酚、4-己基间苯二酚)的高效液相色谱-串联质谱法(HPLC-MS-MS)测定法。方法样品用80%甲醇水溶液超声提取20min,采用LunaC8色谱柱(2mm×100mm,3μm),以0.1%乙酸水溶液-乙腈(含0.1%乙酸)为流动相进行梯度洗脱,流速为0.3ml/min,柱温为35℃。采用电喷雾离子源以负离子多反应监测模式进行质谱监测。结果在0.019~2.60μg/ml的线性范围内,所得4-甲氧基水杨酸钾、苯乙基间苯二酚、二甲氧基甲苯基-4-丙基间苯二酚、4-己基间苯二酚的回归方程均呈较好的线性关系,r>0.999。该方法的检出限为0.21~1.10ng/ml,平均回收率在91.0%~104.7%之间,RSD为1.2%~8.6%。结论该方法高效、快捷、准确,适用于多种化妆品基质中4种美白功效成分的同时快速检测。

Determination of four kinds of whitening efficacy ingredients in cosmetics by high performance chromatography-tandem mass spectrometry

Objective To establish a method for the determination of four kinds of whitening efficacy ingredients,including potassium 4-methoxysalicylate,phenylethyl resorcinol,dimethoxytolyl propylresorcinol,4-hexylresorcinol,in cosmetics by high performance chromatography-tandem mass spectrometry (HPLC-MS-MS).Methods The samples were extracted by 80% methanol aqueous solution under assistance of ultrasonic wave for 20 min and separated on Luna C8 (2 mm×100 mm,3 μm) with 0.1%(V/V) ethylic acid aqueous solution and acetonitrile (containing 0.1% ethylic acid) as the mobile phase for gradient elution.The flow rate was 0.3 ml/min,and the column temperature was 35 ℃.Multiple reaction monitoring (MRM) with negative electrospray ionization (ESI-) in MS-MS was used for quantification.Results In the linear range of 0.019-2.60 μg/ml,the regression equation of four ingredients,including potassium 4 -methoxysalicylate,phenylethyl resorcinol,dimethoxytolyl propylresorcinol,4-hexylresorcinol,showed good linear correlation (r>0.999).The limits of detection were 0.21-1.10 ng/ml.The recoveries of four ingredients were 91.0%-104.7%,with RSDs of 1.2%-8.6%.Conclusion The method is effective,convenient and accurate,and it is applicable to the simultaneous determination of four kinds of whitening efficacy ingredients in various cosmetic substrates in cosmetics.