固相萃取-GC-MS/MS测定化妆品中多种苯甲酸酯类和对苯甲酸酯类防腐剂的含量

Determination of Various Benzoate Esters and p-Benzoate Esters Preservatives in Cosmetics by SPEGC-MS/MS

关键词:  气相色谱-质谱联用  防腐剂  固相萃取  化妆品

Key words:  GC-MS/MS  preservative  solid phase extraction  cosmetics

摘要:

目的 建立同时测定3种不同基质类型(水剂、乳液类和膏霜类)化妆品中苯甲酸乙酯、苯甲酸异丙酯、苯甲酸丙酯、苯甲酸苯基酯、4-羟基苯甲酸甲酯、4-羟基苯甲酸乙酯、4-羟基苯甲酸丁酯和4-羟基苯甲酸丙酯等8种防腐剂的固相萃取-气相色谱-串联质谱(GC-MS/MS)方法。方法 化妆品样品经甲醇提取,采用HLB固相萃取柱净化后检测,经VF-1301MS毛细管柱分离,采用选择离子监测模式(SIM)进行分析,基质匹配标准曲线外标法定量。结果 8种化合物在各自浓度范围内线性关系良好,相关系数均>0.995,检出限为0.079~3.15mg·kg^-1,定量限为0.26~10mg·kg^-1,平均回收率为90.9%~104.2%,RSD均<10%,应用该方法对样品进行了检验。结论 本法简单准确,灵敏度高,可用于市售化妆品中8种防腐剂的定量分析。

Abstract:

OBJECTIVE To establish a gas chromatography tandem mass spectrometry(GC-MS/MS) method for simultaneous separation and determination of eight preservatives including ethyl benzoate, isopropyl benzoate, propyl benzoate,phenyl benzoate, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, butyl 4-hydroxybenzoate and propyl 4-hydroxybenzoate in cosmetics with three different matrix types(water agent, lotion and cream) by solid phase extraction.METHODS Samples were ultrasonically extracted by methanol, then purified by HLB solid phase extraction column. Samples were separated by VF-1301MS capillary column, and analyzed by multi-reaction monitoring(SIM) detection mode. Matrix matching calibration method was used for the quantification.RESULTS The results showed that the eight compounds had good linear relationship in their respective concentration range, the correlation coefficient was > 0.995, the detection limit was 0.079-3.15 mg·kg^-1, the quantitative limit was 0.26-10 mg·kg^-1, and the average recovery was 90.9%-104.2%, RSD was less than 10%, The method was used to test the samples.CONCLUSION The method is simple, accurate and sensitive. It can be used for the quantitative analysis of eight preservatives in commercial cosmetics.