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采用 SPE 与 LC-MS 法测定天然化妆品中的光毒性呋喃香豆素。

Determination of phototoxic furanocoumarins in natural cosmetics using SPE with LC-MS.

机构信息

Institute of Analytical Chemistry and Radiochemistry, CCB-Center for Chemistry and Biomedicine, Leopold-Franzens University of Innsbruck, Innrain 80-82, 6020, Innsbruck, Austria.

ADSI-Austrian Drug Screening Institute GmbH, Innrain 66a, 6020, Innsbruck, Austria.

出版信息

Anal Chim Acta. 2020 Mar 8;1101:211-221. doi: 10.1016/j.aca.2019.12.015. Epub 2019 Dec 9.

DOI:10.1016/j.aca.2019.12.015
PMID:32029113
Abstract

Furanocoumarins are a class of naturally occurring phototoxic substances widely spread throughout the Umbelliferae and Rutacea families of plants. Plant extract of these families (e.g. citrus extracts) are commonly used as ingredients in fragrances and cosmetic products. Due to their phototoxicity these substances are regulated within the European Union according to the European Regulation (EC) No. 1223/2009 on cosmetic products. The proposed analytical workflow aims to swiftly screen out and determine the amount of phototoxic furanocoumarins in natural cosmetics employing solid-phase extraction (SPE). Cosmetic samples were first extracted in methanol and subsequently diluted in 35% (v/v) methanol before being applied to solid-phase extraction. The extraction procedure allows extraction of the eight target compounds including the six marker-substances proposed by the International Fragrance Association (IFRA) from complex cosmetic samples with satisfactory recovery levels ranging from 84 to 116% with the exception of bergamottin (68-89%). HPLC-UV and ESI-MS were used for the analysis of the target compounds. Furanocoumarin quantification was performed by standard addition. The workflow was successfully validated according to the ISO 12787 international standard ("Cosmetics - Analytical methods- Validation criteria for analytical results using chromatographic techniques"). Results of the validation on standard solutions highlight a LOQ of 0.01 mg kg, acceptable linearity up to 1 mg/kg as well as good accuracy (Bias <15%) and precision (RSD <15%). Total furanocoumarin levels of the examined natural cosmetic products were in general in agreement with the European Regulation. However, it was shown that total levels of furanocoumarins might be significantly higher than assumed using the six proposed marker substances only.

摘要

呋喃香豆素是一类广泛存在于伞形科和芸香科植物中的天然光毒性物质。这些科植物的提取物(例如柑橘提取物)通常用作香料和化妆品的成分。由于其光毒性,这些物质根据欧盟关于化妆品的欧洲法规 (EC) No. 1223/2009 进行监管。所提出的分析工作流程旨在使用固相萃取 (SPE) 快速筛选和确定天然化妆品中光毒性呋喃香豆素的含量。首先在甲醇中提取化妆品样品,然后在 35%(v/v)甲醇中稀释,然后再应用于固相萃取。该提取程序允许从复杂的化妆品样品中提取包括国际香料协会 (IFRA) 提出的 6 种标记物质在内的 8 种目标化合物,除了佛手柑内酯(68-89%)外,回收率均达到 84-116%。HPLC-UV 和 ESI-MS 用于分析目标化合物。呋喃香豆素的定量通过标准添加法进行。该工作流程根据国际标准 ISO 12787(“化妆品-分析方法-使用色谱技术分析结果的验证标准”)成功验证。标准溶液的验证结果突出显示,LOQ 为 0.01 mg/kg,线性度可接受,高达 1 mg/kg,并且准确度(偏差<15%)和精密度(RSD<15%)良好。所检查的天然化妆品产品中的总呋喃香豆素水平总体上与欧洲法规一致。然而,结果表明,仅使用 6 种提议的标记物质,总呋喃香豆素水平可能会显著高于预期。

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