高效液相色谱-串联质谱法测定化妆品中的邻苯二甲酸酯

Determination of PAEs in Cosmetic by High Performance Liquid Chromatography-tandem Mass Spectrometry

建立了高效液相色谱-串联质谱（HPLC-MS/MS）法快速测定化妆品中11种邻苯二甲酸酯类化合物的分析方法。化妆品样品经甲醇超声震荡提取,Pro Elut PSA玻璃固相萃取柱净化,采用Endeavorsil C18液相色谱柱分离,以乙腈和水为流动相进行梯度洗脱,采用HPLC-MS/MS进行检测。11种邻苯二甲酸酯类化合物在1~100 ng/m L范围内线性良好（r2=0.999 2）,方法检出限为0.03~0.40 ng/m L,定量限为0.1~1.0 ng/m L,在10、20、50 ng/m L 3个不同加标水平下,平均加标回收率为80.2%~119.4%,相对标准偏差〈15%。该方法有较高灵敏度和精密度,满足化妆品中增塑剂快速检测要求。

A detection method for eleven kinds of PAEs in cosmetic by high performance liquid chromatography-tandem mass spectrometry was established. Various cosmetic samples were extracted by methanol under ultrasonication and purified by the PSA glass solid-phase extraction column,separated on a Endeavorsil C18 liquid chromatographic column with acetonitrile and water as mobile phase,the standard calibration curve for PAEs were in good linearity between the signal strength and the concentration from 1 ~ 100 ng / m L,and the correlation coefficient（ r2） was 0. 999 2. The eleven PAEs limit of detection were 0. 03 ~ 0. 40 ng / m L and the limit of quantification were 0. 1 ~ 1. 0 ng / m L. The mean recoveries of the method for PAEs at three spiked concentration levels of 10,20,50 ng / m L ranged from 80. 2% to 119. 4%,and the relative standard deviations were less than 15%. The proposed method is accurate,sensitive,and is applicable for simultaneous determination of PAEs in cosmetic.