• 中国核心期刊(遴选)数据库收录期刊
  • 中文科技期刊数据库收录期刊
  • 中国期刊全文数据库收录期刊
  • 中国学术期刊综合评价数据库统计源期刊等

中国药物评价 ›› 2019, Vol. 36 ›› Issue (5): 351-353.

• 评价技术与方法 • 上一篇    下一篇

UPLC-MS/MS测定治疗银屑病保健品中甲氨蝶呤的含量

胡珀   

  1. 淮安市食品药品检验所
  • 出版日期:2019-10-28 发布日期:2019-10-28

Quantitative Determination of Methotrexate in the Treatment of psoriasis Health Products by UPLC-MS/MS

  1. Huai''an Institute for Food and Drug Control
  • Online:2019-10-28 Published:2019-10-28

摘要: 目的:建立一种测定治疗银屑病保健品中甲氨蝶呤含量的超高效液相色谱-质谱联用方法。方法:采用Phenomenex Kinetex C18色谱柱(2.1 mm×100 mm,1.7μm),流动相为含0.1%甲酸的水溶液-甲醇,梯度洗脱,流速为0.3 mL·min-1,柱温为 30 ℃;质谱采用电喷雾离子源,多反应监测模式(正离子)。结果:甲氨蝶呤在 0.5~500 μg·L-1内线性关系良好, r为0.999 6,平均回收率为95.67%~98.59%,定量下限为 0.5 μg·L-1,检测限为 0.2 μg·L-1。结论:该方法分析速度快,灵敏度高,结果准确可靠,适用于治疗银屑病保健品中甲氨蝶呤的测定,为打击保健品非法添加提供了有力的技术支撑。

关键词: 超高效液相色谱-质谱联用, 多反应监测, 甲氨蝶呤, 银屑病

Abstract: Objective:To establish a method for the quantitative determination of Methotrexate in the Treatment of psoriasis Health Products by UPLC-MS/MS. Methods: Chromatography was carried on a Phenomenex Kinetex C18(2.1 mm×100 mm,1.7 μm) with the column temperature at 30 ℃, using 0.1% formic acid water solution-methon gradient elution as mobile phase at a flow rate of 0.3 mL·min-1. Determination was performed by multiple reaction monitoring mode using electrospray ionization in positive ion mode. Results:Methotrexate had good linear relationships in 0.5~500 μg·L-1(r=0.999 6), average recoveries were 95.67%~98.59%. The limits of quantitation and detection were 0.5 μg·L-1 and 0.2 μg·L-1, respectively. Conclusion:The method is rapid, sensitive and accurate, and could be an appropriate technique to detect the illegal addition of health products.

Key words: UPLC-MS/MS, Multiple reaction monitoring, Methotrexate, Psoriasis