气相色谱法测定化妆品中的壬二酸

Determination of Azelaic Acid in Cosmetics by Gas Chromatography

采用衍生方式建立了化妆品中壬二酸的样品处理方法,确立了壬二酸衍生物的气相色谱检测方法。结果表明当衍生剂为硫酸和乙醇、衍生时间为1h、衍生温度为70℃时,壬二酸的衍生效果比较好。采用DB-1毛细管色谱柱,升温程序为初温80℃、20℃/min升至300℃后保留3min,壬二酸衍生物能够得到较好分离。用氢火焰离子化检测器检测,外标法定量。壬二酸衍生物在20-1 000mg/L范围内线性关系良好,决定系数r2=0.9996。气相色谱法定性检出限和定量下限分别为50.0和100.0mg/kg,回收率为84.9%-105.8%,RSD〈5%。68批次样品检测结果显示：在标称含有壬二酸的2个样品中,仅有1个检出了壬二酸,其质量比为117mg/kg,其余67种样品均未检出壬二酸。

In this study,agas chromatography method for the determination of azelaic acid in cosmetics was established in derivative way.The results showed that when the derivative agent were sulfuric acid and ethanol,derivative time was 1h,temperature was 70℃,the derivative effect was good.By using DB-1capillary column,when the temperature program was as follows：the initial temperature 80 ℃,at rate of 20 ℃/min to 300 ℃,the retention time 3min,the azelaic acid derivatives could be well separated.The hydrogen flame ionization detector was used and azelaic acid was quantified by external standard method.In the range of 20 to 1 000mg/L,the linear relationship of azelaic acid derivatives were good,the correlation coefficient r2=0.9996,qualitative detection limit was 50.0 mg/kg,quantitative limit was 100 mg/kg.The recovery rate was 84.9% to105.8%,RSD〈5%.The test results of 68 batches of samples showed that only one was detected among 2samples claimed containing azelaic acid,and its mass ratio was 117mg/kg,the other 67 samples were no azelaic acid detected.