高效液相色谱法同时测定化妆品中的19种防晒剂

Simultaneous determination of 19 UV filters in cosmetics by high performance liquid chromatography

目的采用高效液相色谱法建立同时测定不同种类化妆品中19种防晒剂含量的方法。方法样品使用甲醇-四氢呋喃(4∶1)混合溶液提取,经Phenomenex Luna C18色谱柱(4.6 mm×250 mm,5μm)进行分离,流动相A为20%异丙醇的甲醇溶液(含0.1%甲酸),B为0.05%甲酸水溶液,流速为1.2 ml/min,梯度洗脱,以300 nm和350 nm波长作为定量波长,同时进行检测。结果 19种防晒剂校正曲线线性关系良好,r>0.999,4种不同基质中低(60%)、中(100%)、高(140%)3个梯度的加样回收率为95.5%~104.3%,RSD为0.82%~2.45%(n=9),检出限为1 ng^27 ng。本方法与《规范》(2015年版)收载方法具有显著差异。结论本研究所建立的方法流动相低毒、检测结果准确、操作简便,灵敏度高,70批样品测定的结果表明方法具有较高的重现性和耐用性,可用于同时测定化妆品中19种防晒剂含量。

Objective To establish the method for simultaneous determination of 19 UV filters in cosmetics by high performance liquid chromatography（HPLC）. Methods The samples were extracted by mixture of menthol-THF（4 ∶1）,then separated by Phenomenex Luna C18（4. 6 mm × 250 mm,5 μm） column. The mobile phase was A： 20% isopropanol and methanol（containing 0. 1% formic acid）,B： 0. 05% formic acid aqueous solution with gradient elution,the flow rate was 1. 2 ml/min. The detection wavelengths were 300 nm and 350 nm. Results The calibration curves of 19 UV filters showed good linear relationship and the correlation coefficients was above 0. 999. The average recovery at 60%,100%,140% in four different matrixes was within 95. 5%-104. 3%,with RSD of 0. 82%-2. 45%（n = 9）. The detection limit was within 1 ng-27 ng. Conclusion The established method with less toxic mobile phase is accurate,convenient and efficient. The determination results of 70 batches of samples showed that the established method has good reproducibility and durability. It can be used to simultaneously determine 19 UV filters in cosmetics.