高效液相色谱法同时测定化妆品中16种防腐剂、防晒剂和去屑剂  

Simultaneous determination of 16 preservatives,sunscreens and anti-dandruffs in cosmetics by HPLC

作　　者：陈燕 鲍熹珺 闫秀芳 刘建宁 郭芳 牛文霞 Yan Chen;Xijun Bao;Xiufang Yan;Jianning Liu;Fang Guo;Wenxia Niu(Fosun Cosmetics(ShangHai)Bio-Technology Co.,Ltd.,Shanghai 200233,China)

机构地区：[1]星智豫美(上海)生物科技有限公司,上海200233

出　　处：《日用化学工业》2022年第3期337-344,共8页China Surfactant Detergent & Cosmetics

摘　　要：建立了高效液相色谱法同时测定化妆品中防腐剂、防晒剂和去屑剂共16种组分的分析方法。样品经甲醇提取后,使用Eclipse Plus C18(250 mm×4.6 mm×5μm)色谱柱,以甲醇-0.5 mmol/L EDTA-2Na水溶液(pH=3.06)为流动相,梯度洗脱。采用二极管阵列检测器在多波长下同时测定化妆品中10种防腐剂、4种防晒剂和2种去屑剂。该方法的相对标准偏差为2.2%~6.5%,回收率为90.9%~109.7%,16种组分在相应的线性范围内线性关系良好,相关系数范围为0.999 0~0.999 7,该方法具有较高的准确度和精密度,能满足实际检测需求,为实验室检测提供新的技术支持。A method based on HPLC was established for the determination of 16 components in cosmetics including 10 types of preservatives, 4 types of sunscreens and 2 types of anti-dandruffs. The amount of 0.5 g of the cosmetic product was dissolved in methanol in a 10 mL volumetric flask and was ultrasonically extracted for 30 min. The extract was filtered through a 0.22 μm membrane, and then 10 μL solution was introduced onto an Eclipse Plus C18 column(250 mm×0.46 mm×5 μm) with methanol-0.5 mmol/L EDTA-2 Na aqueous solution(pH=3.06) as mobile phase by gradient elution. The 16 components were separated at multiple wavelengths of the DAD detector. These preservatives, sunscreen agents and anti-dandruffs could be analyzed within 50 min simultaneously. The external standard method was employed for quantitative determination. The relative standard deviation of the method is 2.2%-6.5%, and the recovery is 90.9%-109.7%. The limits of detection(LODs, S/N=3) and limits of quantification(LOQs, S/N=10) of 16 components were determined. By this method, different extraction solvent, extraction time and mobile phase were compared. Among these, methanol is used as extraction solvent for 30 minutes and methanol-0.5 mmol/L EDTA-2 Na aqueous solution(pH=3.06) as mobile phase shows good linear relationship in their respective mass concentration range, with the correlation coefficients higher than 0.999 0. This method has high accuracy and precision. 30 products in the market were analyzed, and the results show that phenoxyethanol, benzoic acid, and methyl 4-hydroxybenzoate are the most commonly added preservatives in cosmetics. For the four sunscreens, octyl 4-methoxycinnamate is the most frequently added. Ketoconazole is not detected in these products. In these products, all of the 16 components are lower than the relevant limits in China. This method provides technical support for market supervision and laboratory testing, which also can meet their practical testing requirements.

关 键 词：防腐剂 防晒剂 去屑剂 高效液相色谱法 

分 类 号：TQ658[化学工程—精细化工]