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基质固相分散法分析免洗和冲洗型化妆品中的多类防腐剂。

Analysis of multi-class preservatives in leave-on and rinse-off cosmetics by matrix solid-phase dispersion.

机构信息

Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, Universidad de Santiago de Compostela, Santiago de Compostela, Spain.

出版信息

Anal Bioanal Chem. 2011 Dec;401(10):3293-304. doi: 10.1007/s00216-011-5412-6. Epub 2011 Sep 25.

Abstract

Matrix solid-phase extraction has been successfully applied for the determination of multi-class preservatives in a wide variety of cosmetic samples including rinse-off and leave-on products. After extraction, derivatization with acetic anhydride, and gas chromatography-mass spectrometry analysis were performed. Optimization studies were done on real non-spiked and spiked leave-on and rinse-off cosmetic samples. The selection of the most suitable extraction conditions was made using statistical tools such as ANOVA, as well as factorial experimental designs. The final optimized conditions were common for both groups of cosmetics and included the dispersion of the sample with Florisil (1:4), and the elution of the MSPD column with 5 mL of hexane/acetone (1:1). After derivatization, the extract was analyzed without any further clean-up or concentration step. Accuracy, precision, linearity and detection limits were evaluated to assess the performance of the proposed method. The recovery studies on leave-on and rinse-off cosmetics gave satisfactory values (>78% for all analytes in all the samples) with an average relative standard deviation value of 4.2%. The quantification limits were well below those set by the international cosmetic regulations, making this multi-component analytical method suitable for routine control. The analysis of a broad range of cosmetics including body milk, moisturizing creams, anti-stretch marks creams, hand creams, deodorant, shampoos, liquid soaps, makeup, sun milk, hand soaps, among others, demonstrated the high use of most of the target preservatives, especially butylated hydroxytoluene, methylparaben, propylparaben, and butylparaben.

摘要

基质固相萃取已成功应用于各种化妆品样品中多类防腐剂的测定,包括冲洗型和驻留型产品。萃取后,用乙酸酐衍生化,并进行气相色谱-质谱分析。对真实的未加标和加标驻留型和冲洗型化妆品样品进行了优化研究。通过方差分析(ANOVA)等统计工具以及析因实验设计选择了最适合的提取条件。最终的优化条件对这两组化妆品都适用,包括用 Florisil(1:4)分散样品,以及用 5 mL 正己烷/丙酮(1:1)洗脱 MSPD 柱。衍生化后,无需进一步净化或浓缩步骤即可分析提取物。通过评估准确度、精密度、线性和检测限来评估所提出方法的性能。对驻留型和冲洗型化妆品的回收率研究给出了令人满意的结果(所有样品中所有分析物的回收率均大于 78%),平均相对标准偏差值为 4.2%。定量限远低于国际化妆品法规设定的限值,使得这种多组分分析方法适用于常规控制。对包括身体乳、保湿霜、抗妊娠纹霜、护手霜、除臭剂、洗发水、液体皂、化妆品、防晒乳液、洗手液等多种化妆品的分析表明,大多数目标防腐剂,特别是丁羟甲苯、甲基对羟基苯甲酸酯、丙基对羟基苯甲酸酯和丁基对羟基苯甲酸酯的使用非常广泛。

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