色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 275-281.DOI: 10.3724/SP.J.1123.2014.10029

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法同时测定化妆品中的25种喹诺酮类药物

林黎, 张毅, 涂小珂, 谢丽琪, 岳振峰, 康海宁, 吴卫东, 罗耀   

  1. 深圳出入境检验检疫局食品检验检疫技术中心, 深圳市食品安全检测技术研发重点实验室, 广东 深圳 518045
  • 收稿日期:2014-10-31 修回日期:2015-01-06 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 张毅
  • 基金资助:

    国家自然科学基金项目(21107074);深圳市基础研究项目(JCYJ2012061872144497,JCY201110097).

Determination of 25 quinolones in cosmetics by liquid chromatography-tandem mass spectrometry

LIN Li, ZHANG Yi, TU Xiaoke, XIE Liqi, YUE Zhenfeng, KANG Haining, WU Weidong, LUO Yao   

  1. Food Inspection and Quarantine Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Key Laboratory of Detection Technology Research and Development on Food Safety, Shenzhen 518045, China
  • Received:2014-10-31 Revised:2015-01-06 Online:2015-03-08 Published:2015-02-12

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摘要：

建立了直接提取结合液相色谱-电喷雾串联质谱同时测定化妆品中丹诺沙星、恩诺沙星、氟甲喹、恶喹酸、环丙沙星、沙拉沙星、萘啶酸、诺氟沙星、氧氟沙星等25种喹诺酮类药物的方法。样品经酸性乙腈提取和正己烷脱脂净化,采用Poroshell EC-C18色谱柱分离,含0.1%甲酸的乙腈-水溶液为流动相进行梯度洗脱,电喷雾串联质谱正离子模式扫描,多反应监测(MRM)模式检测,外标法定量。实验通过空白基质液配制标准溶液,以降低基质对离子化干扰造成的基质效应,25种喹诺酮类药物在1~200 mg/kg范围内线性关系良好,相关系数(r)在0.999以上。方法的检出限为1.0 mg/kg,在1、5、10 mg/kg 3个加标水平下,水、乳、霜型化妆品中加标回收率为87.4%~105%,相对标准偏差(RSD)为4.54%~19.7%(n=6)。结果表明,该方法简便、快速、准确,适用于化妆品中25种喹诺酮类药物的测定。

关键词: 化妆品, 喹诺酮, 液相色谱-电喷雾电离串联质谱

Abstract:

An analytical method was developed for the simultaneous determination of 25 quinolones, including danofloxacin mesylate, enrofloxacin, flumequine, oxloinic acid, ciprofloxacin, sarafloxacin, nalidixic acid, norfloxacin, and ofloxacin etc in cosmetics using direct extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Cosmetic sample was extracted by acidified acetonitrile, defatted by n-hexane and separated on Poroshell EC-C18 column with gradient elution program using acetonitrile and water (both containing 0.1% formic acid) as the mobile phases and analyzed by LC-ESI-MS/MS under the positive mode using multiple reaction monitoring (MRM). The interference of matrix was reduced by the matrix-matched calibration standard curve. The method showed good linearities over the range of 1-200 mg/kg for the 25 quinolones with good linear correlation coefficients (r≥0.999). The method detection limit of the 25 quinolones was 1.0 mg/kg, and the recoveries of all analytes in lotion, milky and cream cosmetics matrices ranged from 87.4% to 105% at the spiked levels of 1, 5 and 10 mg/kg with the relative standard deviations (RSD) of 4.54%-19.7%(n=6). The results indicated that this method is simple, fast and credible, and suitable for the simultaneous determination of the quinolones in the above three types of cosmetics.

Key words: cosmetics, liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS), quinolones

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