LC-MS/MS-IDA-EPI法同时测定中草药及中毒样品中16种吲哚生物碱

摘要/Abstract

摘要： 目的建立液相色谱/三重四极杆质谱-多反应监测-信息依赖性采集-增强产物离子扫描（liquid chromatography tandem mass spectrometry-multiple reaction monitoring-information dependent acquisition-enhanced product ion,LC-MS/MS-IDA-EPI）方法,用于同时测定中草药及中毒样品中16种吲哚类生物碱,包括钩吻碱、吴茱萸生物碱、钩藤生物碱、育亨宾和士的宁等。方法用氨水溶液-甲醇（体积分数为0.01%）作为流动相,以0.4 mL/min的流速进行梯度洗脱,16种吲哚类生物碱在Phenomenex Kinetex C₁₈色谱柱上分离。采用多反应监测-信息依赖性采集-增强产物离子（multiple reaction monitoring-information dependent acquisition-enhanced product ion,MRM-IDA-EPI）扫描模式进行检测。结果阳性样品的EPI谱图搜库匹配度均>70%且与标准品的保留时间偏差在±0.1 min内。所有化合物在相应的浓度范围内线性关系良好,相关系数均>0.998,检出限为0.01~4.00（μg/L或μg/kg）,定量限为0.04~13.00（μg/L或μg/kg）。平均回收率为83.43%~109.41%,相对标准偏差（relative standard deviations,RSD）为1.70%~4.51%（n=6）。结论所建立的方法简便快捷、准确、可靠,可用于中草药和中毒样品中16种吲哚类生物碱的快速定性和定量分析。

关键词: 吲哚类生物碱, 液相色谱/三重四极杆质谱, 多反应监测-信息依赖性采集-增强产物离子扫描, 中草药, 中毒样品

Abstract: Objective To establish a liquid chromatography tandem mass spectrometry-multiple reaction monitoring-information dependent acquisition-enhanced product ion（LC-MS/MS-IDA-EPI） method for simultaneous determination of 16 indole alkaloids in Chinese herbal medicine and poisoning samples,including gelsemium elegans alkaloids,evodia rutaecarpa alkaloids,U. rhynchophylla alkaloids,yohimbine,strychnine,etc. Methods The 16 indole alkaloids were separated on a Phenomenex Kinetex C₁₈ column using mobile phases of 0.01% ammonia（v/v） aqueous solution and methanol for gradient elution at a flow rate of 0.4 mL/min. The multiple reaction monitoring-information dependent acquisition-enhanced product ion（MRM-IDA-EPI） scanning modes was used for detection. Results The matching degree of the EPI spectra for the positive samples was greater than 70%,with a deviation in retention time within ±0.1 min. All compounds had good linear relationships within the corresponding concentration range,with correlation coefficients >0.998. The limits of detection and the limit of quantification were 0.01-4.00（μg/L or μg/kg） and 0.04-13.00（μg/L or μg/kg）,respectively. The average recovery rate was 83.43% to 109.41%,and the relative standard deviations（RSD） were 1.70% to 4.51%（n=6）. Conclusion The established method is simple,rapid,accurate,and reliable,and can be used for the rapid qualitative and quantitative analysis of 16 indole alkaloids in Chinese herbal medicine and poisoning samples.

Key words: Indole alkaloids, Liquid chromatography tandem mass spectrometry, Multiple reaction monitoring-information dependent acquisition-enhanced product ion scan, Chinese herbal medicine, Poisoning samples

中图分类号:

R115

黄丽珍, 覃昆飞, 李莜. LC-MS/MS-IDA-EPI法同时测定中草药及中毒样品中16种吲哚生物碱. [J]职业与健康, 2024, 40(18): 2464-2473.

HUANG Lizhen, QIN Kunfei, LI You. Simultaneous determination of 16 indole alkaloids in Chinese herbal medicine and poisoning samples by LC-MS/MS-IDA-EPI method. [J]OCCUPATION AND HEALTH, 2024, 40(18): 2464-2473.

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