成分分析

液质联用法测定齿痛消炎灵颗粒中马兜铃酸Ⅰ和马兜铃内酰胺Ⅰ

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  • 中国食品药品检定研究院,北京 100050
第一作者 刘 静 Tel: (010)67095150;E-mail: liujing_zsm@126.com
刘 阳 Tel: (010)53851571;E-mail: liuyang1819@126.com
*戴 忠 Tel: (010)67095268;E-mail: daizhong@nifdc.org.cn
马双成 Tel: (010)53852076; E-mail: masc@nifdc.org.cn

收稿日期: 2021-04-20

  网络出版日期: 2024-06-24

Analysis of aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules by liquid chromatography-mass spectrometry

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  • National Institutes for Food and Drug Control, Beijing 100050, China

Received date: 2021-04-20

  Online published: 2024-06-24

摘要

目的: 建立齿痛消炎灵颗粒中马兜铃酸Ⅰ和马兜铃内酰胺Ⅰ的液质联用检测分析方法。方法: 采用Agilent SB-C18 (2.1 mm× 50 mm,1.8 μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.3 mL·min-1;多反应监测模式,马兜铃酸Ⅰ为m/z 359.0→298.1(定量)和m/z 359.0 → 296.1(定性),马兜铃内酰胺Ⅰ为m/z 294.0 → 278.9(定量)和m/z 294.0→251.1(定性),建立齿痛消炎灵颗粒中2个马兜铃酸类成分的液质联用检测方法,在方法学验证的基础上对所有样品进行检测分析。结果: 马兜铃酸Ⅰ和马兜铃内酰胺Ⅰ进样量分别在51.849~1 036.984、1.842~36.848 pg范围内线性关系良好,R2≥ 0.999 5,定量限分别为26.91、0.69 pg,平均加样回收率分别为107.2%~107.4%(RSD 0.50%~2.1%)、98.9%~105.5%(RSD 1.3%~2.9%)。16批齿痛消炎灵颗粒样品中均未检出马兜铃酸Ⅰ,马兜铃内酰胺Ⅰ的检出量为0.063~0.763 μg·g-1结论: 所建立的方法准确、灵敏、可靠,能够用于齿痛消炎灵颗粒中上述马兜铃酸类成分的筛查与分析,为其安全性有关成分研究提供科学依据。

本文引用格式

刘静, 刘阳, 武营雪, 戴忠, 马双成 . 液质联用法测定齿痛消炎灵颗粒中马兜铃酸Ⅰ和马兜铃内酰胺Ⅰ[J]. 药物分析杂志, 2022 , 42(2) : 237 -242 . DOI: 10.16155/j.0254-1793.2022.02.07

Abstract

Objective: To establish the analysis method of aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules by liquid chromatography-mass spectrometry (LC-MS). Methods: An Agilent SB-C18 (2.1 mm× 50 mm,1.8 μm) column was used with gradient elution of acetonitrile-0.1% formic acid at a flow rate of 0.3 mL·min-1. The multiple-reaction monitoring mode was used and the detection ion pairs for aristolochic acid Ⅰ were m/z 359.0→ 298.1 (quantitation), m/z 359.0 → 296.1 (qualitation) for aristolochic acid Ⅰ, and m/z 294.0 → 278.9 (quantitation), m/z 294.0 → 251.1 (qualitation) for aristolactam Ⅰ . As a result, the LC-MS method was established to detect the aristolochic acid Ⅰ and aristolactam Ⅰ in Chitong Xiaoyanling granules. And the method was further validated and used to test all samples. Results: The developed method showed good linearity in the range of 51.849-1 036.984 pg and 1.842-36.848 pg with R2≥0.999 5 for aristolochic acid Ⅰ and aristolactam Ⅰ, respectively. The limits of quantification (LOQs) were 26.91 and 0.69 pg, and the average recovery rates were 107.2%-107.4% (RSD 0.5%-2.1%), 98.9%-105.5% (RSD 1.3%-2.9%), respectively. Aristolochic acid Ⅰ was not detected in all the 16 batches of samples. And the conetens of aristolactam Ⅰ were in the range of 0.063-0.763 μg·g-1. Conclusion: The established method is accurate, sensitive and reliable. It can be applied for analysis of aristolochic acid analogues in Chitong Xiaoyanling granules. And it can provide sound scientific basis for the study of safety related components.

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