液相色谱–串联质谱法测定化妆品中的β-苔黑酚酸甲酯

Determination of methyl atratate in cosmetics by liquid chromatography–tandem mass spectrometry

建立水剂、乳液、膏霜、香波、油脂5种化妆品基质中β-苔黑酚酸甲酯的液相色谱–串联质谱测定方法。样品用甲醇提取,乳液和香波样品用弱阴离子小柱净化;用C18色谱柱分离,流动相为乙腈–水,梯度洗脱;质谱仪为电喷雾离子源–串联四级杆质谱;采用选择反应监测模式。β-苔黑酚酸甲酯的质量浓度在0.5~10μg/L范围内与色谱峰面积呈良好的线性,线性相关系数(r2)为0.999,方法检出限为3μg/kg,定量限为10μg/kg。5种基质3个浓度水平平均加标回收率为83.0%~108%,测定结果的相对标准偏差为0.8%~7.3%(n=6)。方法快速、准确,适合化妆品中β-苔黑酚酸甲酯的测定。

A method for determining methyl-atratate in water,lotion,cream,shampoo and oil cosmetics by liquid chromatography–tandem mass spectrometry was established. Samples were extracted by methanol. Lotion and shampoo samples was cleaned by WAX cartridges. A C18 column was used for separation with acetonitrile–water as the mobile phase,gradient elution was selected. An electrospray–tandem quadrupole mass spectrometry and select reaction monitoring were used. The concentration of methyl atratate was linear with the chromatographic peak area in the range of 0.5–10 μg/L. The linear correlation coefficient(r2) was 0.999. The detection limit was 3 μg/kg and the quantification limit was 10 μg/kg. The meant recoveries in five matrixes at three concentration levels ranged from 83.0% to 108%. The relative standard deviations of detection results were 0.8%–7.3%(n=6). The method is accurate and quick,which is suitable for the determination of methyl atratate in cosmetics.