提出了高效液相色谱-串联质谱法测定化妆品中二甲胺、二乙胺、乙醇胺、二乙醇胺、三乙醇胺、二甲基乙醇胺、二乙基乙醇胺等7种乙醇胺类化合物含量的方法。样品经体积比1∶9的0.005 mol·L^-1乙酸铵溶液-乙腈混合液提取后,过滤,滤液注入高效液相色谱-串联质谱仪。以Agilent InfinityLab Poroshell 120 HILIC-Z 色谱柱(100 mm×2.1 mm,2.7 μm)为固定相,以不同体积比的0.005 mol·L^-1乙酸铵溶液-乙腈混合液为流动相进行梯度洗脱;分离后的7种目标物经电喷雾离子源正离子模式扫描,动态多反应监测模式检测。结果显示:7种乙醇胺类化合物质量浓度在一定范围内与定量离子峰面积呈线性关系,检出限(3S/N)为0.09~5.39 ng·g^-1;按照标准加入法对水基类、乳基类和霜基类共3种类型的阴性样品进行回收试验,回收率为88.0%~115%,测定值的相对标准偏差(n=6)均小于6.0%;方法用于20批化妆品分析,其中17批化妆品中均未检出目标物,3批化妆品中检出三乙醇胺,质量分数为0.17%~1.0%。

A method for the determination of 7 ethanolamine compounds including dimethylamine, diethylamine, ethanolamine, diethanolamine, triethanolamine, dimethylethanolamine and diethyl ethanolamine in cosmetics by high performance liquid chromatography-tandem mass spectrometry was proposed. The sample was extracted by the mixed solution composed of 0.005 mol·L^-1 ammonium acetate solution and acetonitrile at volume ratio of 1∶9. After filtration, the filtrate was injected into a high performance liquid chromatography-tandem mass spectrometer. Gradient elution was performed on Agilent InfinityLab Poroshell 120 HILIC-Z column (100 mm×2.1 mm, 2.7 μm) as stationary phase, with the mixed solutions composed of 0.005 mol·L^-1 ammonium acetate solution and acetonitrile at different volume ratios as mobile phase. The 7 separated targets were scanned by electrospray ion source with positive ion mode, and detected by dynamic multi-reaction monitoring mode. It was shown that linear relationships between the mass concentrations and peak areas of quantitative ions for 7 ethanolamine compounds were kept in definite ranges, with detection limits (3S/N) in the range of 0.09-5.39 ng·g^-1. Test for recovery was made on the three kinds of negative samples including water base, milk base and cream base by standard addition method, giving results in the range of 88.0%-115%,with RSDs (n=6) of the determined values were less than 6.0%. The method was applied to analysis of 20 batches of cosmetics, among which targets were not detected in 17 batches of cosmetics, and triethanolamine was detected in 3 batches of cosmetics, with mass fractions in the range of 0.17%-1.0%.