山东科学 ›› 2019, Vol. 32 ›› Issue (3): 118-122.doi: 10.3976/j.issn.1002-4026.2019.03.018

• 其他研究论文 • 上一篇    

液相色谱-质谱联用测定不同软膏中的莫匹罗星

胡玉芬,王丽娟,薛富民*   

  1. 齐鲁工业大学(山东省科学院),山东省分析测试中心,山东 济南 250014
  • 收稿日期:2018-08-08 出版日期:2019-06-20 发布日期:2019-06-01
  • 通信作者: 薛富民(1979—),男,博士,研究方向为食品及环境中有害物质分析检测技术。E-mail:xuefm@sdas.org E-mail:xuefm@sdas.org
  • 作者简介:胡玉芬(1978—),女,硕士,研究方向为食品及环境中有害物质分析检测技术。E-mail:yufenne@163.com
  • 基金资助:
    山东省重点研发计划(2018GSF117006)

Determination of mupirocin in different ointments by HPLC-MS

HU Yu-fen, WANG Li-juan, XUE Fu-min*   

  1. Qilu University of Technology (Shandong Academy of Sciences), Shandong Analysis and Test Center, Jinan 250014, China
  • Received:2018-08-08 Online:2019-06-20 Published:2019-06-01

摘要: 建立了一种液相色谱-质谱联用测定不同软膏中莫匹罗星含量的方法。色谱柱为Agilent XDB-C18(2.1 mm×50 mm,1.8 μm);水相为 0.1 %甲酸-水,有机相为乙腈,梯度洗脱,流速为 0.3 mL·min-1,柱温30 ℃。采用ESI 离子源正离子模式,多反应离子监测模式下选择离子对501.3→326.7、501.3→308.9和501.3→291.0进行测定。结果表明,莫匹罗星检测质量浓度线性范围为10~500 ng·mL-1r=0.999 5);检出限和定量限分别为4、10 ng·mL-1,精密度实验的相对标准偏差(n=6)为0.8%;低、中、高浓度的加标回收率(n=3)分别为99.8%、109.2% 和105.0% ,相对标准偏差(n=3)分别为3.5%、1.6%和1.4%。该方法灵敏度高、专属性好、精密度高、简便、快速,可用于不同软膏中莫匹罗星的检测。

关键词: 莫匹罗星, 液相色谱-质谱联用, 灵敏度, 专属性

Abstract: A method for the determination of mupirocin in different ointments by the high performance liquid chromatography-mass spectrometry (HPLC-MS) was established. The analytical column was Agilent XDB-C18(2.1 mm × 50 mm,1.8 μm), the mobile phase was 0.1% formic acid solution and acetonitrile with gradient elution, and the flow rate was 0.3 mL·min-1. The column temperature was set at 30 ℃. The detection was achieved in ESI positive ion mode with 501.3→326.7, 501.3→308.9 and 501.3→291.0. Results showed that the calibration curve was in a linearity over the range of 10~500 ng·mL-1(r=0 .999 5). The limit of detection and quantification was 4 ng·mL-1and 10 ng·mL-1, respectively. Precision was fine, with RSD(n=6)of 0.8%. The recoveries(n=3)of low, middle and high adding concentrations were 99.8%, 109.2% and 105.0%,and the RSD(n=3) were 3.5%, 1.6% and 1.4%, respectively. The established method is sensitive, specific, accurate, simple and rapid, which is applicable for the determination of mupirocin in different ointments.

Key words: mupirocin, HPLC-MS, sensitivity, specialization

中图分类号: 

  • R917