欢迎访问《日用化学工业(中英文)》,今天是

日用化学工业(中英文) ›› 2026, Vol. 56 ›› Issue (10): 1413-1418.doi: 10.3969/j.issn.2097-2806.2026.10.014

• 分析与检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定牙膏中7种止血药

张丽媛1,程巧鸳1,*(),陈紫怡2,陈帅霖2,戚绿叶1,黄柳倩1   

  1. 1 浙江省食品药品检验研究院 全省生物医药接触材料重点实验室, 浙江 杭州 310052
    2 浙江药科职业大学, 浙江 宁波 315100
  • 收稿日期:2025-12-12 修回日期:2026-09-22 出版日期:2026-10-22 发布日期:2026-10-30
  • 基金资助:
    浙江省药品监管科技计划项目(2025011);中央引导地方科技发展资金项目(2025ZY01093)

Simultaneous determination of seven hemostatic drugs in toothpaste by high performance liquid chromatography-tandem mass spectrometry

Liyuan Zhang1,Qiaoyuan Cheng1,*(),Ziyi Chen2,Shuailin Chen2,Lvye Qi1,Liuqian Huang1   

  1. 1 Zhejiang Key Laboratory of Biopharmaceutical Contact Materials, Zhejiang Institute for Food and Drug Control, Hangzhou, Zhejiang 310052, China
    2 Zhejiang Pharmaceutical University, Ningbo, Zhejiang 315100, China
  • Received:2025-12-12 Revised:2026-09-22 Online:2026-10-22 Published:2026-10-30
  • Contact: E-mail: chengqiaoyuan@zjyj.org.cn

摘要:

建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定牙膏中氨甲环酸等7种止血药含量的方法。样品经5%甲醇-0.02 mmol/L乙二胺四乙酸二钠溶液超声提取后,采用Agilent Poroshell 120 Aq-C18色谱柱(2.1 mm×150 mm,2.7 μm) 分离,以0.1%甲酸-甲醇为流动相进行梯度洗脱,电喷雾离子源(ESI),正、负离子多反应监测(MRM)模式定量。结果显示,在相应的质量浓度范围内,7种止血药相关系数(R2)均高于0.998,线性关系良好。检出限(LOD)为0.05~3.73 μg/g,定量限(LOQ)为0.17~12.30 μg/g。在低、中、高3个质量浓度水平下,2种牙膏基质样品中7种止血药的加标回收率为87.5%~111.9%,相对标准偏差为0.6%~4.4% (n=6)。该方法操作简便、准确度好、灵敏度高,适用于多基质牙膏中7种止血药的测定。

关键词: 牙膏, 止血药, 氨甲环酸, 高效液相色谱-质谱联用法, 基质效应

Abstract:

A method for the simultaneous determination of seven hemostatic drugs in toothpaste was developed using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted ultrasonically with 5% methanol-0.02 mmol/L disodium ethylenediaminetetraacetate solution. The analytes were separated on an Agilent Poroshell 120 Aq-C18 column (2.1 mm×150 mm, 2.7 μm) column via gradient elution with 0.1% formic acid-methanol as mobile phase. Quantitative analysis was performed by electronic spray ionization under a positive ion and negative ion mode with multiple reaction monitoring (MRM). The results indicate that the seven hemostatic drugs show good linearity within their respective concentration ranges, with correlation coefficients (R2) greater than 0.998. The limits of detection are 0.05~3.73 μg/g, and the limits of quantitation are 0.17~12.30 μg/g. The average spiked recoveries of the seven hemostatic drugs in two toothpaste matrices are all in the range of 87.5%~111.9%, with RSDs of 0.6%~4.4% (n=6). The method is simple, sensitive and accurate, making it suitable for the routine determination of these hemostatic drugs in toothpaste.

Key words: toothpaste, hemostatic drugs, tranexamic acid, HPLC-MS/MS, matrix effect

中图分类号: 

  • TQ658