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日用化学工业（中英文）

日用化学工业 ›› 2016, Vol. 46 ›› Issue (11): 661-664.doi: 10.13218/j.cnki.csdc.2016.11.010

• 分析与检测 • 上一篇    下一篇

液相色谱-串联质谱法测定祛痘化妆品中5种硝基咪唑类化合物

张鑫鑫1,2,高媛惠3,花锦3,杨燕强2,申迎华1   

  1. 1.太原理工大学 化学化工学院,山西 太原 030024;
    2.长治出入境检验检疫局,山西 长治 046000;
    3.山西出入境检验检疫局,山西 太原 030024
  • 出版日期:2016-11-22 发布日期:2019-04-18
  • 作者简介:张鑫鑫(1983-),女,山西高平人,工程师,硕士研究生,电话:13623556821,E-mail:zhangxin168188@sina.com。

Determination of five kinds of nitroimidazole compound in whelk dispelling cosmetics by liquid chromatography- tandem mass spectrometry

ZHANG Xin-xin1,2,GAO Yuan-hui3,HUA Jin3,YANG Yan-qiang2,SHEN Ying-hua1   

  1. 1.School of Chemistry and Chemical Engineering,Taiyuan University of Technology,Taiyuan,Shanxi 030024,China;
    2.Changzhi Entry-Exit Inspection and Quarantine Bureau,Changzhi,Shanxi 046000,China;
    3.Shanxi Entry-Exit Inspection and Quarantine Bureau,Taiyuan,Shanxi 030024,China
  • Online:2016-11-22 Published:2019-04-18

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摘要： 采用液相色谱-串联质谱(LC-MS/MS)法建立了测定祛痘化妆品中5种硝基咪唑类化合物(甲硝唑(MNZ)、洛硝哒唑(RNZ)、二甲硝咪唑(DMZ)、羟基甲硝唑(MNZOH)和1-甲基-5-硝基-2-羟甲基咪唑(HMMNI))的方法。样品经乙酸乙酯提取,采用Hypersil GOLD C18色谱柱(2.1 mm×100 mm,3 μm)分离,依次用丙酮、甲醇和V(氨水)∶V(乙腈)=5∶95的混合溶液淋洗,采用LC-MS/MS在多反应监测(MRM)正离子模式下检测,基质外标法定量。结果表明:MNZ,RNZ和DMZ在0~50 μg/L内呈良好线性关系,MNZOH和HMMNI在0~100 μg/L内呈良好线性关系;5种硝基咪唑药物线性相关系数R2>0.99;在试样中进行3个水平的加标回收实验,平均回收率为84.3%～115.0%,相对标准偏差(RSD)为1.66%～10.30% (n=6),适用于祛痘化妆品中硝基咪唑类化合物的检测和确证需要。

关键词: 祛痘化妆品, 硝基咪唑类化合物, 液相色谱-串联质谱

Abstract: A method for determination of five kinds of nitroimidazole compound (metronidazole (MNZ),ronidazole (RNZ),dimetridazole (DMZ),hydroxyl metronidazole (MNZOH) and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI)) in whelk dispelling cosmetics by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established.The target analyte was extracted from the product sample with ethyl acetate as solvent,and the extract was separated on a Hypersil GOLD C18 column (2.1 mm×100 mm,3 μm),sequentially eluted with acetone,methanol and blend solution with V(ammonia water)∶V(acetonitrile)=5∶95,detected using LC-MS/MS in the multiple reaction monitoring (MRM) positive ion mode,and quantified by external standard matrix method.The results indicated that good linearity displays when mass concentration of MNZ,RNZ and DMZ is within 0~50 μg/L,and when mass concentration of MNZOH and HMMNI is within 0~100 μg/L.Linear correlation coefficient (R2) is higher than 0.99.In the spiked test of three levels,the average recovery rate is in the range of 84.3%-115.0%,and relative standard deviation (RSD) is in the range of 1.66%-10.30% (n=6).This analysis method meets the testing requirements for detection and confirmation.

Key words: whelk dispelling cosmetics, nitroimidazole compound, liquid chromatography-tandem mass spectrometry

中图分类号: 

  • TQ658