LC-MRM3法测定中草药和药酒中3种强心作用的生物碱

摘要/Abstract

摘要： 目的建立液相色谱-多级多反应监测模式（liquid chromatography-multiple-reaction monitoring cubed,LC-MRM³）同时测定中草药和药酒中3种强心作用的生物碱（欧夹竹桃苷、欧夹竹桃苷乙和去甲乌药碱）。方法样品用80%甲醇提取后经30%乙腈稀释后直接进样,在Phenomenex Kinetex C₁₈色谱柱（100×2.1 mm,2.6 μm）上进行梯度洗脱,分离后采用LC-MRM³模式检测。结果 3种生物碱在相应的浓度范围内呈良好的线性关系（r>0.999）,药酒样品检出限为0.019~0.071 μg/L,草药样品检出限为0.006~0.022 μg/kg,加标回收率为90.31%~97.92%,相对标准偏差为1.14%~2.73%（n=6）。与传统的液相色谱-多反应监测模式（liquid chromatography-multiple-reaction monitoring,LC-MRM）方法相比,LC-MRM³方法的检测灵敏度提升约一个数量级,并且允许简单的样品制备,而不会有基质效应的影响。定性结果通过多级串联质谱（multi-stage mass spectrometry,MS³）扫描得到进一步确认。LC-MRM³的定量结果与LC-MRM的结果基本一致。结论该方法简便、快速、可靠,可用于同时检测中草药和药酒中3种强心作用的生物碱。

关键词: 欧夹竹桃苷, 欧夹竹桃苷乙, 去甲乌药碱, 液相色谱-多级多反应监测模式

Abstract: Objective To establish a liquid chromatography-multiple-reaction monitoring cubed（LC-MRM³） methods for the simul-taneous determination of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor（Oleandrin,Adynerin and Higenamine）. Methods The samples were extracted with 80% methanol,diluted with 30% acetonitrile,and then directly injected. Gradient elution was performed on a Phenomenex Kinetex C₁₈ chromatographic column（100×2.1 mm,2.6 μm）,and after separation, detected using the LC-MRM³ mode. Results The three alkaloids showed good linear relationships within their respective concentration ranges（r>0.999）. The detection limits in medicinal liquor samples ranged from 0.019 to 0.071 μg/L,for Chinese herbal medicine samples,the detection limits ranged from 0.006 to 0.022 μg/kg. The spike recovery rate was 90.31%-97.92%,with a relative standard deviation of 1.14%-2.73%（n=6）. Compared to the traditional method liquid chromatography-multiple-reaction monitoring（LC-MRM）,the LC-MRM³ method enhanced the detection sensitivity by an order of magnitude and allowed for simple sample preparation without the impact of matrix effects. Qualitative results were further confirmed through multi-stage mass spectrometry（MS³） scanning. The quantitative results of LC-MRM³ were essentially consistent with those of LC-MRM. Conclusion This method is simple,fast,and accurate,and can be used for the simultaneous detection of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor.

Key words: Oleandrin, Adynerin, Higenamine, LC-MRM³

中图分类号:

R115

覃昆飞, 黄丽珍, 何建忠. LC-MRM³法测定中草药和药酒中3种强心作用的生物碱. [J]职业与健康, 2024, 40(17): 2337-2345.

QIN Kunfei, HUANG Lizhen, HE Jianzhong. Simultaneous determination of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor using LC-MRM³ method. [J]OCCUPATION AND HEALTH, 2024, 40(17): 2337-2345.

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LC-MRM³法测定中草药和药酒中3种强心作用的生物碱

Simultaneous determination of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor using LC-MRM³ method

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