中国药物警戒 ›› 2023, Vol. 20 ›› Issue (4): 388-391.
DOI: 10.19803/j.1672-8629.20220163

• 基础与临床研究 • 上一篇    下一篇

纸喷雾离子化质谱快速筛查复杂基质中的西格列汀

宋东宁, 刘静Δ, 张才煜, 刘阳#, 何兰, 张庆生*   

  1. 中国食品药品检定研究院,国家药品监督管理局化学药品质量研究与评价重点实验室,北京 102629
  • 收稿日期:2022-04-14 出版日期:2023-04-15 发布日期:2023-04-20
  • 通讯作者: *张庆生,男,主任药师,药物质量管理。Email: zqs@nifdc.org.cn;#为共同通信作者。
  • 作者简介:宋东宁,女,在读硕士,药物分析。Δ为并列第一作者。
  • 基金资助:
    国家重点研发计划(2016YFE0205400); 国家药品监督管理局化学药品质量研究与评价重点实验室课题(2021-5)

Rapid detection of sitagliptin in complex matrices by paper spray ionization mass spectrometry

SONG Dongning, LIU JingΔ, ZHANG Caiyu, LIU Yang#, HE Lan, ZHANG Qingsheng*   

  1. National Institutes for Food and Drug Control, NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs, Beijing 102629, China
  • Received:2022-04-14 Online:2023-04-15 Published:2023-04-20

摘要: 目的 建立一种用于快速筛查复杂基质中西格列汀的纸喷雾离子化质谱(PSI-MS)方法。方法 采用 PSI-MS 技术,优化喷雾电压、喷雾溶剂、色谱纸尖至质谱锥孔距离、进样方式等实验参数,对复杂基质中的西格列汀进行快速筛查,并通过内标法进行半定量分析。结果 每个样品检测时间小于1 min,西格列汀在0.1~10 μg·mL-1范围内线性关系良好,相关系数 r2 为0.999 8,加样回收率实验结果在 94%~109%,并且RSD均小于5%。结论 本方法操作简便、前处理简单、灵敏度高、重现性好,可用于复杂基质中西格列汀的快速识别及定量。

关键词: 纸喷雾离子化, 质谱, 西格列汀, 快速筛查, 复杂基质, 降血糖药

Abstract: Objective To establish an analytical method based on paper spray ionization mass spectrometry (PSI-MS) for rapid screening of sitagliptin in complex matrices. Methods Such experimental parameters as the spray voltage, spray solvent, distance from the tip of the chromatographic paper to the injection port of the mass spectrometer were optimized. A semi-quantitative method for rapid characterizing sitagliptin was established by adding an internal standard. Results Sitagliptin could be detected in less than one minute. The linear relationship of this method was good and the correlation coefficient r2 was 0.999 8 within the range of 0.1 to 10 μg·mL-1. The recovery rates were between 94% and 109% with an RSD of less than 5%. Conclusion This method is simple, user-friendly, sensitive and precise, which can be used to quantitatively determine the content of sitagliptin in complex matrices.

Key words: paper spray ionization, mass spectrometry, sitagliptin, rapid determination, complex matrix, antidiabetic medicine

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