高效液相色谱法检测防晒类化妆品中的尿刊酸及其乙酯

doi:10.13218/j.cnki.csdc.2016.04.012

摘要/Abstract

摘要： 研究建立了同时测定防晒类化妆品中尿刊酸及其乙酯的高效液相色谱检测方法及质谱确证方法。化妆品样品以甲醇为提取溶剂进行超声提取,提取液经离心处理、微孔滤膜过滤后测定。采用XTerra MS C₁₈色谱柱(4.6 mm×250 mm,5 μm)进行分离,以甲醇-5 mmol/L四丁基溴化铵溶液(体积比为30∶70)为流动相进行等梯度洗脱,流速为1.0 mL/min,柱温为35 ℃,检测波长为285 nm,外标法定量。防晒类化妆品中尿刊酸及其乙酯的方法定量限均为5 mg/kg,在低、中、高3个添加水平范围内平均回收率为80.1%~103.8%,相对标准偏差(RSD)为1.2%~6.9%。对于疑似阳性的样品,进一步采用液相色谱-串联质谱法进行确证分析。该方法准确、快速、灵敏度高,适用于防晒类化妆品的实际检验工作。

关键词: 防晒化妆品, 尿刊酸, 尿刊酸乙酯, 高效液相色谱

Abstract: A high performance liquid chromatography (HPLC) was established for the simultaneous determination of urocanic acid and its ethyl ester in sunscreen cosmetics.The result was comfirmed with mass spectrometry.Cosmetic samples were extracted with methanol under assistance of ultrasonic wave and the extract was centrifuged and filtered with a microporous membrane filter.Then the filtrate was transfer for HPLC analysis using an XTerra MS C₁₈ column (4.6 mm×250 mm,5 μm).The mobile phase was a solution composed of methanol and 5 mmol/L tetrabutylammonium bromide (30∶70) with isocratic elution.The column temperature was set at 35 ℃.The flow rate was 1 mL/min and the wavelength of detection was at 285 nm.The quantification was carried out by external standard method.The experimental results indicated that the limits of quantification (LOQs) for urocanic acid and its ethyl ester were both 5 mg/kg.The mean recoveries at three spiked levels ranged from 80.1% to 103.8% with the relative standard deviations (RSD) between 1.2% and 6.9%.The suspected positive samples were subjected to further verification by LC-MS/MS.The method is accurate,rapid,sensitive,and can be used for the inspection of sunscreen cosmetics.

Key words: sunscreen cosmetics, urocanic acid, ethyl urocanate, high performance liquid chromatography

中图分类号:

TQ658.2+4

郭项雨,马强,孟宪双,李焘,李文雅,白桦. 高效液相色谱法检测防晒类化妆品中的尿刊酸及其乙酯[J]. 日用化学工业, 2016, 46(4): 238-242.

GUO Xiang-yu,MA Qiang,MENG Xian-shuang,LI Tao,LI Wen-ya,BAI Hua. Determination of urocanic acid and its ethyl ester in sunscreen cosmetics by HPLC[J]. China Surfactant Detergent & Cosmetics, 2016, 46(4): 238-242.

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