气相色谱-质谱联用测定化妆品中硫酸二甲酯与硫酸二乙酯

建立了同时测定化妆品中硫酸二甲酯和硫酸二乙酯的气相色谱-质谱(GC-MS)联用法。样品经溶剂提取后采用GC-MS测定,外标法定量。水基类、乳液类、膏霜类、啫喱类和粉类化妆品的方法检出限均为1.5 mg/kg,定量下限均为5.0 mg/kg;蜡基类化妆品的检出限为3.0 mg/kg,定量下限为10.0 mg/kg;油状化妆品的方法检出限为5.0 mg/kg,定量下限为16.0 mg/kg。目标物在0.25~20.0 mg/L范围内线性良好,相关系数均大于0.99,硫酸二甲酯的平均回收率为83.8%~104.7%,相对标准偏差为2.7%~8.2%;硫酸二乙酯的平均回收率为84.7%~104.8%,相对标准偏差为3.5%~8.7%。方法前处理简单,灵敏度高,可满足水基类、乳液类、膏霜类、啫喱类、粉类和油状化妆品中硫酸二甲酯和硫酸二乙酯的检测要求。

Determination of Dimethyl Sulfate and Diethyl Sulfate in Cosmetics by GC-MS

A new method was developed for the determination of dimethyl sulfate and diethyl sulfate in cosmetics by gas chromatography-mass spectrometry(GC-MS).After extracted with solvent,the samples were determined by GC-MS and quantified by external standard method.The MDLs and MLOQs for the cosmetics(water-based,emulsions,creams,gel and powder),the wax cosmetics and the oiliness cosmetics were 1.5,5.0 mg/kg,3.0,10.0 mg/kg and 5.0,16.0 mg/kg,repectively.There existed a good linearity for the analyte in the concentration range of 0.25-20.0 mg/L with the correlation coefficients larger than 0.99.The recoveries of dimethyl sulfate and diethyl sulfate were in the ranges of 83.8%-104.7% and 84.7%-104.8% with their RSDs of 2.7%-8.2% and 3.5%-8.7%,respectively.The optimized method was accurate,rapid and sensitive,and was suitable for the determination of dimethyl sulfate and diethyl sulfate in cosmetics(water-based,emulsions,creams,gel,powder,wax-base and oiliness ).