色谱 ›› 2015, Vol. 33 ›› Issue (12): 1327-1332.DOI: 10.3724/SP.J.1123.2015.06042

• 技术与应用 • 上一篇    下一篇

高效液相色谱法测定化妆品中11种二苯酮类紫外线吸收剂

曲宝成, 边海涛, 毛希琴, 李劲   

  1. 大连市食品检验所, 辽宁 大连 116630
  • 收稿日期:2015-06-24 出版日期:2015-12-08 发布日期:2012-06-21
  • 通讯作者: 毛希琴

Measurement of 11 benzophenone ultraviolet-filters in cosmetics by high performance liquid chromatography

QU Baocheng, BIAN Haitao, MAO Xiqin, LI Jin   

  1. Dalian Institute of Food Inspection, Dalian 116630, China
  • Received:2015-06-24 Online:2015-12-08 Published:2012-06-21

摘要:

建立了化妆品中11种二苯酮类紫外线吸收剂的高效液相色谱分析方法。采用四氢呋喃-甲醇-水或二氯甲烷-水体系提取化妆品中二苯酮类紫外线吸收剂,经离心(5000 r/min),上清液过0.22 μm滤膜后,进入高效液相色谱分析。采用C18色谱柱进行分离,以0.1% (体积分数)甲酸水溶液(含10 mmol/L乙酸铵)为流动相A,以0.1% (体积分数)甲酸甲醇为流动相B,梯度洗脱。方法加标回收率(n=7)为93.4%~103.8%,相对标准偏差为0.1%~4.2%,方法的检出限为4.0~30 μg/g,方法的定量限为15~100 μg/g。采用该方法对42种市售化妆品检测分析发现,有5种二苯酮类紫外线吸收剂被检出,其中防晒隔离液中二苯酮-3和香水中二苯酮-2的检出量分别为2785 μg/g和2106 μg/g。研究结果表明,所建立的方法具有良好的回收率、重现性和较高的灵敏度,可用于化妆品中多种二苯酮类紫外线吸收剂的分析。

关键词: 二苯酮类, 高效液相色谱, 化妆品, 紫外线吸收剂

Abstract:

A sample preparation and analytical method with liquid-liquid extraction (LLE) and high performance liquid chromatography (HPLC) was developed to detect 11 benzophenone ultraviolet-filters in cosmetics. The target compounds were extracted by the mixed solutions of tetrahydrofuran (THF)/methanol/water or dichloromethane/water at proper ratios. The extracts were centrifuged and filtered to remove matrix compounds, and then analyzed by HPLC. The separation of analytes was carried out on a Diamonsil-C18 column (150 mm×4.6 mm, 5 μm) with 0.1%(v/v) formic acid aqueous solution (containing 10 mmol/L ammonium acetate) as mobile phase A and methanol containing 0.1%(v/v) formic acid as mobile phase B. The spiked recoveries of the method (n=7) were 93.4%-103.8% with the relative standard deviations of 0.1%-4.2%. The limits of detection (LODs) were in the range of 4.0-30 μg/g and the limits of quantitation (LOQs) ranged from 15 to 100 μg/g. The method was applied to the determination of 42 cosmetic samples randomly purchased from the supermarket in Dalian. Five benzophenone series were always detected, in which the content of benzophenone-3 in sunscreen cream and the content of benzophenone-2 in perfume were very high and reached 2785 μg/g and 2106 μg/g, respectively. The results showed that the developed method is efficient, reliable and sensitive, which can be applied to the determination of benzophenones in cosmetics.

Key words: benzophenone series, cosmetics, high performance liquid chromatography (HPLC), ultraviolet-filters

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