色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 450-453.DOI: 10.3724/SP.J.1123.2011.00450

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时检测口腔卫生用品中的硝基咪唑类药物

徐娟*, 陈捷, 邵琳智, 李荀   

  1. 广东出入境检验检疫局, 广东 广州 510623
  • 收稿日期:2011-01-12 修回日期:2011-03-01 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 徐娟,硕士,工程师.
  • 基金资助:
    国家检验检疫行业标准制定计划项目(No. 2009B100)

Determination of nitroimidazoles in oral hygiene by ultra-performance liquid chromatography-tandem mass spectrometry

XU Juan*, CHEN Jie, SHAO Linzhi, LI Xun   

  1. Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
  • Received:2011-01-12 Revised:2011-03-01 Online:2011-05-28 Published:2011-05-28

PDF

515

被引次数

34

摘要： 建立了采用超高效液相色谱-串联质谱同时检测口腔卫生用品(牙膏及漱口水)中甲硝唑、替硝唑、奥硝唑、二甲硝咪唑和洛硝唑的方法。试样以0.1%(体积分数)的甲酸水溶液/乙腈(95:5, v/v)稀释,经高速离心后过滤膜净化,采用Cloversil C18色谱柱(100 mm×2.1 mm, 3.5 μm)分离,以0.1%甲酸水溶液和乙腈为流动相梯度洗脱,质谱检测,外标法定量。5种硝基咪唑类化合物在1.0～60.0 μg/L质量浓度范围内线性关系良好,相关系数r均不小于0.9992;在10.0、20.0和100 mg/kg加标水平的平均回收率为91.5%～108%,相对标准偏差为1.14%～5.22%;方法的定量限(LOQ,以信噪比为10计)为2.0 mg/kg。该方法可靠、稳定,可满足口腔卫生用品中硝基咪唑类药物含量检测与确证的需要。

关键词: 超高效液相色谱-串联质谱法, 口腔卫生用品, 硝基咪唑类药物

Abstract: A method for the simultaneous determination of metronidazole, tinidazole, ornidazole, ronidazole and dimetridazole in oral hygiene by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed. The sample was diluted with 0.1% formic acid/acetonitrile (95:5, v/v), then centrifuged and filtered with a membrane. The separation was carried out on a Cloversil C18 column (100 mm×2.1 mm, 3.5 μm) with the gradient elution of 0.1% formic acid and acetonitrile as the mobile phases. The analytes were determined by UPLC-MS/MS and quantified by external standard method. The calibration curves showed good linearity in the range of 1.0~60.0 μg/L with r≥0.9992. The recoveries were 91.5%~108% at the three spiked levels of 10.0, 20.0 and 100 mg/kg, and the relative standard deviations were 1.14%~5.22%. This method is easy, sensitive and suitable for the determination of nitroimidazoles in oral hygiene.

Key words: nitroimidazoles, oral hygiene, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)