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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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QuEChERS-液相色谱-串联质谱法快速测定肝细胞癌血液中3种小分子代谢物

Rapid determination of three small-molecule metabolites in the hepatocellular carcinoma blood using QuEChERS-liquid chromatography-mass spectrometry

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (5):830-838
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:通过建立QuEChERS(快速、简易、廉价、有效、稳定、安全)前处理方法,结合液相色谱-三重四极杆质谱联用技术,实现肝细胞癌血液中3种小分子代谢物的同时检测。方法:血清样品经乙腈提取,无水硫酸镁盐析及N-丙基乙二胺(PSA)吸附剂净化后,取上清液采用Phenomenex Luna Omega 3 μm PS C18 100&#197;(150 mm&#215;2.1 mm)色谱柱,以甲醇-0.1%乙酸水溶液为流动相,梯度洗脱。电喷雾离子源正离子扫描,多反应监测模式(MRM)进行定量分析。结果:十四酰胺的检测下限为0.6 ng&#183;g-1,定量下限为2 ng&#183;g-1;油酸酰胺的检测下限为0.3 ng&#183;g-1,定量下限为1 ng&#183;g-1。3种小分子代谢物质量浓度在10~100 ng&#183;mL-1范围内呈线性,其中目标物线性相关系数(R2)均大于0.991 7,基质效应(ME)在0.79~1.55之间;3个水平加样回收率在77.5%~105.1%之间,日内精密度(n=5)在6.9%~11.8%之间,日间精密度在7.4%~11.1%之间;利用该方法扩大样本量检测,3种小分子代谢物在健康组血清中的浓度(2.591、0.221、7.485 mg&#183;kg-1)和肝癌组血清中的浓度(9.599、0.266、5.063 mg&#183;kg-1)差异显著(P<0.01)。结论:该方法简单快捷,准确可靠,适合于大批量肝细胞癌血液样品中3种小分子代谢物的快速检测。

-----英文摘要:---------------------------------------------------------------------------------------

Objective:To establish an LC-MS method for the simultaneous determination of 3 small-molecule metabolites in the hepatocellular carcinoma blood by establishing quEChERS (quick, easy, cheap, effective, rugged, safe) coupled with liquid chromatography-mass spectrometer.Methods:Serum samples were extracted with acetonitrile and anhydrous sodium sulfate were used for salting-out process.After purified by PSA, the supernatant was applied on a Phenomenex Luna Omega 3 μm PS C18 100&#197; (150 mm&#215;2.1 mm) column with methanol-0.1% acetic acid solution as mobile phase and subjected to gradient elution.For quantitation, electrospray ionization (ESI) source was applied and the mass spectrometer was operated in multiple reaction monitoring (MRM) modes. Results:The limits of detection (LOD) and the limits of quantification (LOQ) for n-tetradecanamide were 0.6 ng&#183;g-1 and 2 ng&#183;g-1 respectively.LOD and LOQ for oleamide were 0.3 ng&#183;g-1 and 1 ng&#183;g-1 respectively.There was a good linear relationship in the range of 10-100 ng&#183;mL-1 of the 3 small-molecule metabolites.The target linear correlation coefficient (R2) was higher than 0.991 7.The matrix effect (ME) was between 0.79 and 1.55.The method recovery was between 77.5% and 105.1% in three spike levels.The intraday precision (n=5) was between 6.9% and 11.8% and daytime precision was between 7.4% and 11.1%.Using this method to expand the sample size detection, the concentration of three small-molecule metabolites in healthy group (2.591, 0.221, 7.485 mg&#183;kg-1) and cancer group (9.599, 0.266, 5.063 mg&#183;kg-1) were significantly different (P<0.01).Conclusion:This method is simple, accurate and reliable, and is suitable for the rapid detection of three small-molecule metabolites in large quantities of the hepatocellular carcinoma blood samples.

-----参考文献:---------------------------------------------------------------------------------------

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