色谱

色谱 ›› 2013, Vol. 31 ›› Issue (5): 416-422.DOI: 10.3724/SP.J.1123.2012.12006

• 研究论文 • 上一篇    下一篇

化妆品中8种呋喃香豆素的高效液相色谱法检测及质谱确证

马会娟1, 马强1*, 李文涛1, 孟宪双1, 李晶瑞1, 白桦1, 焦阳2, 张晓丽2   

  1. 1. 中国检验检疫科学研究院, 北京 100123;
    2. 国家质量监督检验检疫总局 国际检验检疫标准与技术法规研究中心, 北京 100028
  • 收稿日期:2012-12-03 修回日期:2013-01-21 出版日期:2013-05-28 发布日期:2013-05-16
  • 通讯作者: 马强,Tel:(010)85773279,E-mail:maqiang1129@yahoo.com.cn.
  • 基金资助:

    质检公益性行业科研专项项目(2012104013-4);国家科技支撑计划项目(2013BAK04B03);国家质量监督检验检疫总局科技计划项目(2011IK196);国家标准化管理委员会计划项目(20101088-T-607).

Simultaneous determination of eight furocoumarines in cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry

MA Huijuan1, MA Qiang1*, LI Wentao1, MENG Xianshuang1, LI Jingrui1, BAI Hua1, JIAO Yang2, ZHANG Xiaoli2   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    2. Research Center for International Inspection and Quarantine Standard and Technical Regulation, General Administration of Quality Supervision, Inspection and Quarantine, Beijing 100028, China
  • Received:2012-12-03 Revised:2013-01-21 Online:2013-05-28 Published:2013-05-16

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摘要：

建立了同时测定化妆品中8种呋喃香豆素类化合物(8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、三甲沙林、欧前胡素和异欧前胡素)的高效液相色谱分析方法及液相色谱-串联质谱确证方法。膏霜类、水剂类、香波类、散粉类、唇膏类等不同类型的化妆品样品分别经适宜的提取溶液进行超声提取,提取液以离心处理后,取上清液经微孔滤膜过滤后测定。采用Agilent Zorbax SB-Phenyl色谱柱(250 mm×4.6 mm, 5 μm)分离,以甲醇-乙腈-水三元流动相梯度洗脱,流速1.0 mL/min,柱温30 ℃,检测波长250 nm。8-羟基补骨脂素的定量限为0.25 mg/kg,补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、三甲沙林、欧前胡素、异欧前胡素的定量限为0.5 mg/kg。在低、中、高3种加标水平下,8种待测组分的平均回收率为85.0%～105.8%,相对标准偏差为0.41%～7.90%。采用本方法在一日内不同时间点(6个时间点,每隔1 h测定一次)和不同日期(6 d内)测定混合标准溶液,得到8个目标物峰面积的日内精密度均小于1%,日间精密度均小于2%。该方法准确、简便、快速,适用于不同类型化妆品中8种呋喃香豆素类化合物的测定。

关键词: 呋喃香豆素, 高效液相色谱, 化妆品, 液相色谱-质谱/质谱

Abstract:

A method using high performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of eight furocoumarines (8-hydroxypsoralen, psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin) in cosmetics. The cosmetic samples, including cream, lotion, shampoo, powder and lipstick, were supersonically extracted with appropriate solvents. The extract was centrifuged, and the supernatant was filtered through a membrane, and then separated on an Agilent Zorbax SB-Phenyl chromatographic column (250 mm×4.6 mm, 5 μm) by gradient elution at a flow rate of 1.0 mL/min with methanol-acetonitrile-water as mobile phases. The column temperature was set at 30 ℃. The wavelength of detection was 250 nm. The limits of quantification (LOQs) were 0.25 mg/kg for 8-hydroxypsoralen and 0.5 mg/kg for psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin. The recoveries at three spiked levels were in the range of 85.0%-105.8% with the relative standard deviations (RSDs) of 0.41%-7.90%. The intra-day precision (n=6) was less than 1%, and the inter-day precision (n=6) was less than 2% for the peak areas of the eight furocoumarines in a mixed standard solution. The method is accurate, simple, rapid and suitable for the determination of the eight furocoumarines in various cosmetic samples.

Key words: cosmetics, furocoumarines, high performance liquid chromatography (HPLC), liquid chromatography-tandem mass spectrometry (LC-MS/MS)

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