液相色谱-紫外及荧光检测法测定化妆品中的对羟基苯甲酸酯类

Determination of p-hydroxybenzoic acid esters in cosmetics by liquid chromatography with ultraviolet and fluorescence detection.

作者信息

Akimoto N, Yamamoto M, Sato S, Masui T, Narita H

机构信息

Shizuoka Prefectural Institute of Public Health and Environmental Science, Japan.

出版信息

J Assoc Off Anal Chem. 1988 Jul-Aug;71(4):823-5.

PMID:3417609

Abstract

A simple, precise, and accurate liquid chromatographic method with both ultraviolet (UV) and fluorescence detection is described for the determination of methyl, ethyl, propyl, and butyl p-hydroxybenzoates (PHBA-esters) in cosmetics. sec-Butyl p-hydroxybenzoate is added to the sample as an internal standard. Then the PHBA-esters are extracted with ether, the ether is evaporated to dryness, and the residue is dissolved in 60% (v/v) acetonitrile. The acetonitrile solution is passed through a Sep-Pak C18 cartridge to remove co-extracted lipids. PHBA-esters are determined by reverse-phase liquid chromatography with UV detection at 254 nm and fluorescence detection at ex 280 nm, em 305 nm. The mobile phase is acetonitrile-water (35 + 65). The method was linear over the concentration range of 0.005-0.15 mg/mL. Mean recoveries of each PHBA-ester were 98.9-102.7% (coefficients of variation less than or equal to 2.0%).

摘要

本文描述了一种简单、精确且准确的液相色谱法，该方法采用紫外（UV）和荧光检测，用于测定化妆品中的对羟基苯甲酸甲酯、乙酯、丙酯和丁酯（PHBA酯）。将对羟基苯甲酸仲丁酯作为内标加入样品中。然后用乙醚萃取PHBA酯，将乙醚蒸发至干，残余物溶于60%（v/v）乙腈中。乙腈溶液通过Sep-Pak C18柱以去除共萃取的脂质。采用反相液相色谱法在254 nm处进行紫外检测，在激发波长280 nm、发射波长305 nm处进行荧光检测来测定PHBA酯。流动相为乙腈 - 水（35 + 65）。该方法在0.005 - 0.15 mg/mL的浓度范围内呈线性。各PHBA酯的平均回收率为98.9 - 102.7%（变异系数小于或等于2.0%）。