论文部分内容阅读
建立了超高效液相色谱-串联质谱法(UHPLC-MS-MS)同时测定化妆品中21种性激素含量的分析方法。水状、乳状、油状的化妆品采用甲醇/乙腈(1∶1,V/V)漩涡提取,利用HLB固相萃取柱净化萃取,选取4 m L乙腈为洗脱液收集样品液后,经C18色谱柱分离,以甲醇-乙腈及0.5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用动态多反应监测(d MRM)扫描方式进行测定。21种性激素成分在25~800 ng/m L范围内呈良好的线性关系,其相关系数(r2)均大于0.999,方法定量限(LOQs)为0.05~0.61 mg/kg。此外,高、低两个浓度加标水平的实验结果表明,方法平均回收率为74%!110%,相对标准偏差(RSD)为1.2%~10%(n=3)。
A method for the simultaneous determination of 21 sex hormones in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS) was established. The aqueous, milky and oily cosmetics were extracted by swirling methanol / acetonitrile (1: 1, V / V), HLB solid phase extraction column, 4 mL acetonitrile was chosen as eluent, The column was separated and eluted with methanol-acetonitrile and 0.5 mmol / L ammonium acetate as mobile phase. The mobile phase was monitored by dynamic multi-reaction monitoring (d MRM). The linear relationship of 21 sex hormones in the range of 25 ~ 800 ng / m L was obtained. The correlation coefficients (r2) were all above 0.999. The LOQs were between 0.05 and 0.61 mg / kg. In addition, the experimental results of high and low concentration spike levels showed that the average recovery was 74% ~ 110% and the relative standard deviation (RSD) was 1.2% ~ 10% (n = 3).