色谱

色谱

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超高效液相色谱-串联质谱法分析化妆品中的常见抗生素及甲硝唑

刘华良1*,李放1,杨润1,王联红2,马永建1   

  1. 1.Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China; 2.State Key Laboratory of Pollution Control and Resources Reuse, School of the Environment, Nanjing University, Nanjing 210093, China
  • 收稿日期:2008-06-30 修回日期:2008-10-02 出版日期:2009-01-30 发布日期:1983-03-25
  • 通讯作者: 刘华良
  • 基金资助:
    国家科技支撑计划项目 (No. 2006BAK02A01).

Determination of common antibiotics and metronidazole in cosmetics by ultra performance liquid chromatography-tandem mass spectrometry

LIU Hualiang1*, LI Fang1, YANG Run1, WANG Lianhong2, MA Yongjian1   

  1. 1.Jiangsu Provincial Center for Disease Control and Prevention, Nanjing 210009, China; 2.State Key Laboratory of Pollution Control and Resources Reuse, School of the Environment, Nanjing University, Nanjing 210093, China
  • Received:2008-06-30 Revised:2008-10-02 Online:2009-01-30 Published:1983-03-25
  • Contact: LIU Hualiang

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1283

被引次数

31

摘要： 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定化妆品中常见的6种抗生素(美满霉素、土霉素、四环素、金霉素、多西环素、氯霉素)及甲硝唑的方法,并用于实际样品的分析。样品经甲醇-0.1 mol/L甲酸溶液(体积比为1∶1)超声提取后,以甲醇(含1%甲酸)-水(含1%甲酸)为流动相,经UPLC梯度洗脱分离后以多反应监测(MRM)模式质谱测定。方法的检出限为3～20 ng/g,回收率为87%～101%,工作曲线的线性相关系数大于0.995,线性范围为2～1000 μg/L (达3个数量级)。对11份市售化妆品进行分析检测,其中2份检出氯霉素,质量分数分别为0.37%和0.19%;1份检出甲硝唑,质量分数为1.02%;美满霉素、土霉素、四环素、金霉素、多西环素未检出。

关键词: 超高效液相色谱-串联质谱法, 化妆品 , 甲硝唑, 抗生素

Abstract: A method for the analysis of common antibiotics and metronidazole in cosmetics was developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). One gram of each cosmetic sample was extracted by methanol-water containing 0.1 mol/L formic acid (1∶1, v/v). The extracted sample was filtered before being analyzed with UPLC/MS/MS. The effects of formic acid concentration in the mobile phase on the sensitivity and retention time were studied, and the results showed that 1% was the optimum concentration. Seven analytes, minocycline, oxytetracycline, tetracycline, chlortetracycline, doxycycline, chloramphenicol, metronidazole, can be separated and detected in 5 min, which is much faster than that by the conventional liquid chromatography. The detection limits were 3-20 ng/g, and the recoveries were 87%-101%. The calibration curves showed good linearity in the range of 2-1000 μg/L with correlation coefficients larger than 0.995. The method was also applied to determine common antibiotics and metronidazole in 11 real samples from themarket. Chloramphenicol was detected in 2 samples and the concentrations were 0.37% and 0.19%; metronidazole was detected in 1 sample and the concentration was 1.02%; others were not detected.

Key words: antibiotics, cosmetics , metronidazole, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)