安全监测

高分离度快速液相色谱-三重串联四极杆质谱快速检查消渴灵片中山麦冬*

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  • 广西壮族自治区食品药品检验所,南宁 530021
第一作者 Tel:13597179437;E-mail: 137968757@qq.com
** 林燕翔 Tel:13878197214;E-mail:1062619725@qq.com
罗 轶 Tel:13877171269;E-mail:luoyi20010211@163.com

收稿日期: 2020-02-24

  网络出版日期: 2024-05-31

基金资助

* 广西重点研发计划“广西常用壮瑶药药材质量标准研究”(桂科 AB17292069); 南宁市科技基地专项“广西南宁市中药材检测科技创新示范中心”(20191035)

Rapid test of Liropes Radix in Xiaokeling tables by rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry*

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  • Guangxi Zhuang Autonomous Region Food and Drug Control, Nanning 530021, China

Received date: 2020-02-24

  Online published: 2024-05-31

摘要

目的:建立消渴灵片中山麦冬的专属性检测方法。方法: 样品经甲醇-氨水超声提取,利用高分离度快速液相色谱-三重串联四极杆质谱(RRLC-QQQ/MS)检测山麦冬。采用 Thermo Accla imTM RSLC 120 C18 色谱柱(2.1 mm×100 mm,1.8 μm),以乙腈(A)-20 mmol·L-1乙酸铵溶液(B)为流动相,梯度洗脱(0~20 min,5%A → 90%A),流速 0.2 mL·min-1,柱温 30 ℃,进样量 2 μL。离子化模式为 ESI+,选择 m/z 723.4 → 251.2 和 m/z 723.4 → 269.2 作为山麦冬皂苷 B 检测离子对,m/z 893.5 → 463.1 和 m/z 893.5 → 481.2 作为短葶山麦冬皂苷 C 检测离子对,进行多反应监测。结果:山麦冬皂苷 B 和短葶山麦冬皂苷 C 的检测下限分别为 0.28 μg·片 -1 和 0.20 μg·片 -1。111 批次消渴灵片中有 8 家企业的 25 批样品掺伪,其中 6 批次样品同时掺入湖北麦冬和短葶山麦冬,4 批次样品为湖北麦冬掺伪,15 批次样品为短葶山麦冬掺伪。结论:所建方法专属、准确、快速、简便,可为消渴灵片的专项治理提供有力的技术支持。

本文引用格式

黄博, 姚力, 张慧, 张颖婷, 林燕翔, 罗轶 . 高分离度快速液相色谱-三重串联四极杆质谱快速检查消渴灵片中山麦冬*[J]. 药物分析杂志, 2021 , 41(2) : 320 -328 . DOI: 10.16155/j.0254-1793.2021.02.16

Abstract

Objective:To establish a method for the specific detection of Liriopes Radix in Xiaokeling tablets. Methods:The samples were extracted by methanol-ammonia,rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry(RRLC-QQQ/MS)was used to detect Liriopes Radix. The Thermo AcclaimTMRSLC 120 C18(2.1 mm×100 mm,1.8 μm)column was used.Acetonitrile -20 mmol·L-1ammonium acetate solution was used as mobile phase,and gradient elution(0~20 min,5%A → 90%A),flow rate was 0.2 mL·min-1.Column temperature was 30 ℃,injection was 2 μL.The ionized mode was ESI+,and m/z 723.4 → 251.2 and m/z 723.4 → 269.2 were selected as the ion pairs of liriopeside B,and m/z 893.5 → 463.1 and m/z 893.5 → 481.2 as the ion pairs of Liriope muscari Baily saponin C,for multi-reaction monitoring. Results:The detection limits of liriopeside B and Liriope muscari Baily saponin C were 0.28 μg per tablet and 1.50 μg per tablet, respectively.6 batches of samples from batch 111 Xiaokeling tablets were mixed with Liriope spicata var.prolifera Y.T.Ma and Liriope muscari(Decne.)Bailey,4 batches of samples were adulterated with Liriope spicata var. prolifera Y.T.Ma,and 15 batches of samples were adulterated with Liriope muscari(Decne.)Bailey,involving 25 batches of samples from 8 enterprises. Conclusion:The established method is accurate,rapid and simple,which can provide strong technical support for the special treatment of Xiaokeling tablets.

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