高效液相色谱-蒸发光散射法同时测定化妆品和牙膏中6种多羟基化合物  

Simultaneous determination of six polyhydroxyl compounds in cosmetics and toothpaste using high performance liquid chromatography with evaporative light-scattering detection

作　　者：赵淑娥 袁璐 廖丹丹 罗香 肖庚鹏 ZHAO Shu’e;YUAN Lu;LIAO Dandan;LUO Xiang;XIAO Gengpeng(Development Research Institute of Testing and Certification Technology,Jiangxi General Institute of Testing and Certification,Nanchang 330029,China)

机构地区：[1]江西省检验检测认证总院检测认证技术发展研究院,江西南昌330029

出　　处：《色谱》2025年第3期269-274,共6页Chinese Journal of Chromatography

基　　金：江西省市场监督管理局科技项目(GSJK202125,GSJK202126).

摘　　要：建立了同时测定化妆品和牙膏中玻色因、木糖醇、山梨醇、甘露醇、蔗糖、肌醇等6种多羟基化合物的方法。水可分散样品和水包油样品用水提取,提取液再经乙酸乙酯和正己烷洗涤;油包水样品先用乙酸乙酯预分散,再用水提取,最后提取液经正己烷洗涤。提取液经Ultimate XB-NH 2柱(250 mm×4.6 mm,5μm)分离,乙腈-水溶液梯度洗脱,蒸发光散射检测器检测,外标法定量。分别对提取过程和色谱条件等进行了优化。在优化的实验条件下,6种多羟基化合物在0.2~5.0 g/L范围内线性关系良好,相关系数为0.991~0.996;方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.10%和0.35%。针对水包油、油包水的化妆品和牙膏基质,进行了低、中、高3个水平的加标回收试验,目标物的平均回收率为84.7%~94.1%,相对标准偏差(RSD,n=6)为2.2%~6.9%。该方法具有经济简便、稳定可靠、重复性好等优势,适用于化妆品中多羟基化合物的检测。With the full implementation of the cosmetic formula ingredient registration system and the standardized management of labels and identification,the ingredients registered and declared on the label must be consistent with the actual ingredients contained in the product.Further,cosmetic manufacturers require accurate determination of the ingredients in cosmetics for formula analysis.Therefore,a method for the simultaneous determination of six polyhydroxyl compounds,Pro-Xylane,xylitol,sorbitol,mannitol,sucrose,and inositol,in cosmetics and toothpaste was established.According to this method,approximately 0.5 g of the sample was weighed into a 25 mL centrifuge tube.Water-dispersed and oil-in-water cosmetic samples were extracted using 10 mL water,followed by washing with 5 mL n-hexane and 5 mL ethyl acetate.The water-in-oil cosmetic samples were predispersed in 5 mL ethyl acetate,extracted using 10 mL water,and washed with 5 mL n-hexane.After filtration through a 0.22μm membrane,the extracted solution was subjected to separation using an Ultimate XB-NH 2 column(250 mm×4.6 mm,5μm),employing gradient elution with acetonitrile and distilled water as the mobile phases.This was followed by detection using evaporative light-scattering detector(ELSD)and quantification using the external standard method.Optimization experiments were conducted to select chromatographic columns,extraction processes,and chromatographic conditions.Specifically,the Ultimate XB-NH 2 column and Ultimate XB-C 18 column were compared in terms of separation efficiency.Based on the separation efficiency and analysis time,the XB-NH 2 column was found to be more suitable as the separation column for this method.The effects of trichloromethane(TCM),ethyl acetate(EA),and n-hexane as predispersants and washing solutions were compared.Among them,the combination of ethyl acetate and n-hexane was found to be more suitable owing to its effective pre-dispersion capability and ability to remove both polar and nonpolar compounds from the extraction solution.Th

关 键 词：高效液相色谱 蒸发光散射检测 多羟基化合物 化妆品 牙膏 

分 类 号：O658[理学—分析化学]