Liang Jing, Zhuang Wan'e, Wei Danqi, Ou Yan, Gong Zhenbin
State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361005, China.
Se Pu. 2012 Mar;30(3):273-9. doi: 10.3724/sp.j.1123.2011.11022.
A method was developed for the simultaneous determination of 19 phthalate esters (PAEs) at trace level in cosmetics by solid phase extraction (SPE) purification and gas chromatography-mass spectrometry (GC-MS) detection. The PAEs were extracted from cosmetic samples by dichloromethane with ultrasonic-assisted technique, purified by an SPE column packed with silica gel and neutral alumina (2: 3, m/m) with the elution of 20 mL of mixed solvent of ethyl acetate-hexane (8: 2, v/v). Qualitative and quantitative analysis were carried out by GC-MS in full scan and selected ion monitoring modes. The retention time of quantitative ions and the abundance ratio of characteristic ions were applied to rapidly and accurately identify each analyte so as to prevent the occurring of possible mistakes from complex matrix intervention. Under optimized conditions, the average recoveries for a shampoo sample spiked with the standards at 0.1, 0.5, 2.0 microg/g were in the range of 72.2% and 110.9%, and the relative standard deviations (RSDs) for the 19 PAEs were less than 10.3% (n = 6) at the spiked level of 0.1 microg/g. The limits of detection (LODs, as 3 times of standard deviation) were between 0.0065 microg/g (for diisopentyl phthalate) and 0.062 microg/g (for diisobutyl phthalate). The method was successfully applied to the determination of the PAEs in 6 types of cosmetics. It is expected to promote the determination of the PAEs in other cosmetics with different matrices.
建立了一种通过固相萃取(SPE)净化和气相色谱 - 质谱联用(GC - MS)检测同时测定化妆品中19种痕量邻苯二甲酸酯(PAEs)的方法。采用二氯甲烷超声辅助技术从化妆品样品中萃取PAEs,通过填充硅胶和中性氧化铝(2:3,m/m)的SPE柱进行净化,用20 mL乙酸乙酯 - 己烷混合溶剂(8:2,v/v)洗脱。采用GC - MS在全扫描和选择离子监测模式下进行定性和定量分析。利用定量离子的保留时间和特征离子的丰度比快速准确地鉴定各分析物,以防止复杂基质干扰导致可能的错误发生。在优化条件下,对于添加了0.1、0.5、2.0 μg/g标准品的洗发水样品,平均回收率在72.2%至110.9%之间,在0.1 μg/g加标水平下,19种PAEs的相对标准偏差(RSDs)小于10.3%(n = 6)。检测限(LODs,以3倍标准偏差计)在0.0065 μg/g(邻苯二甲酸二异戊酯)至0.062 μg/g(邻苯二甲酸二异丁酯)之间。该方法成功应用于6种化妆品中PAEs的测定,有望推动不同基质其他化妆品中PAEs的测定。