高效液相色谱/三重四极杆质谱联用法测定血浆和尿液中鹅膏肽类毒素

引用本文: 魏佳会, 陈佳, 吴弼东, 陈作红, 吴剑峰, 谢剑炜. 高效液相色谱/三重四极杆质谱联用法测定血浆和尿液中鹅膏肽类毒素[J]. 分析化学, 2020, 48(3): 405-412. doi: 10.19756/j.issn.0253-3820.191604 shu

Citation: WEI Jia-Hui, CHEN Jia, WU Bi-Dong, CHEN Zuo-Hong, WU Jian-Feng, XIE Jian-Wei. Determination of Amanita Peptides in Human Plasma and Urine by High-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2020, 48(3): 405-412. doi: 10.19756/j.issn.0253-3820.191604 shu

高效液相色谱/三重四极杆质谱联用法测定血浆和尿液中鹅膏肽类毒素

1.
军事科学院军事医学研究院毒物药物研究所, 抗毒药物与毒理学国家重点实验室, 北京 100850;
2.
中国人民解放军第五医学中心, 北京 100071;
3.
湖南师范大学生命科学学院, 长沙 410081

摘要: 建立了高效液相色谱/三重四极杆质谱联用法测定人体血浆及尿液样本中3类5种鹅膏肽类毒素的分析方法。样品经固相萃取分离富集后，在CAPCELL CORE C₁₈色谱柱上分离，流动相为10 mmol/L乙酸铵-甲醇，采用梯度洗脱分离，正离子多反应监测模式（MRM）检测。血浆和尿液样品中5种鹅膏肽类毒素在较宽浓度范围内均呈良好线性关系，检出限为0.2和0.5 μg/L （S/N=3）；加标回收率分别为98.0%~114.6%和90.1%~99.4%，准确度、精密度及基质效应等均符合方法学要求。本方法操作简便、分析速度快、灵敏度高，并被应用于鹅膏菌中毒实际样本中鹅膏肽类毒素的检测，为中毒病人的及时救治提供了准确、可靠的技术支持。

关键词:

English

Determination of Amanita Peptides in Human Plasma and Urine by High-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

1.
State Key Laboratory of Toxicology and Medical Countermeasures and Laboratory of Toxicant Analysis, Institute of Pharmacology and Toxicology, Academy of Military Medical Sciences, Beijing 100850, China;
2.
PLA 307 Hospital, Beijing 100071, China;
3.
College of Life Sciences, Hunan Normal University, Changsha 410081, China
Received Date: 14 October 2019
Revised Date: 31 December 2019

Abstract: Five amanita peptide toxins, such as α-amanita, β-amanita, phalloidin, viroidin and ala-viroidin in human plasma and urine were determined by high-performance liquid chromatography coupled with triple quadrupole mass spectrometry under positive ion multiple reaction monitoring mode (MRM). The samples were enriched and purified by HLB solid phase extraction cartridge, and separated by CAPCELL CORE C₁₈ column using 10 mmol/L aqueous ammonium acetate-methanol as mobile phase under a gradient elution. The results indicated that the five amanita peptide toxins in plasma or urine had good linear relationship in a wide range of concentration levels. The detection limits of the toxins were 0.2 and 0.5 μg/L (S/N=3), the average recoveries were 98.0%-114.6% and 90.1%-99.4% for spiked plasma and urine samples, respectively. Accuracy, precision and matrix effects could meet the methodological requirement for biological samples analysis. The established method had many advantages such as simple operation and high sensitivity, which provided an accurate and reliable technical support for the diagnosis and medical treatment of clinical amanita poisoned patients.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

高效液相色谱/三重四极杆质谱联用法测定血浆和尿液中鹅膏肽类毒素

English

Determination of Amanita Peptides in Human Plasma and Urine by High-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

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