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1.山西医科大学 法医学院,山西 晋中 030600
2.公安部鉴定中心,北京 100038
3.中国人民公安大学 侦查学院,北京 100038
4.法庭毒物分析公安部重点实验室,北京市公安司法鉴定中心,北京 100192
王瑞花,硕士,研究员,研究方向:毒物分析,E-mail:nqkczs@126.com
收稿日期:2025-01-14,
修回日期:2025-02-20,
录用日期:2025-02-28,
纸质出版日期:2025-07-15
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金珊珊,常靖,吴世豪,董林沛,辛国斌,王瑞花.UPLC-MS/MS法同时测定血液中儿茶酚胺及其代谢物[J].分析测试学报,2025,44(07):1378-1384.
JIN Shan-shan,CHANG Jing,WU Shi-hao,DONG Lin-pei,XIN Guo-bin,WANG Rui-hua.Simultaneous Determination of Catecholamines and Their Metabolites in Blood by UPLC-MS/MS Method[J].Journal of Instrumental Analysis,2025,44(07):1378-1384.
金珊珊,常靖,吴世豪,董林沛,辛国斌,王瑞花.UPLC-MS/MS法同时测定血液中儿茶酚胺及其代谢物[J].分析测试学报,2025,44(07):1378-1384. DOI: 10.12452/j.fxcsxb.25011426.
JIN Shan-shan,CHANG Jing,WU Shi-hao,DONG Lin-pei,XIN Guo-bin,WANG Rui-hua.Simultaneous Determination of Catecholamines and Their Metabolites in Blood by UPLC-MS/MS Method[J].Journal of Instrumental Analysis,2025,44(07):1378-1384. DOI: 10.12452/j.fxcsxb.25011426.
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定血液中儿茶酚胺(CAs)
及其3种代谢物的检测方法。该方法仅需100 µL血样,经超滤离心管净化,固相萃取法提取,采用HSS PFP色谱柱分离,以乙腈-0.1%甲酸水溶液作为流动相梯度洗脱。电喷雾正离子多反应监测(MRM)模式检测,内标法定量。结果表明,CAs及其代谢物在0.5~50 ng/mL质量浓度范围内线性良好(
r
2
>
0.99),方法检出限和定量下限分别为0.2 ng/mL和0.5 ng/mL。6种目标物在1、10、50 ng/mL 3个加标水平下的回收率为68.9%~101%,基质效应为 86.2%~102%,相对标准偏差(RSD)为2.3%~10%。所建方法为临床诊断、肾上腺素中毒案件的检验鉴定提供了有效的技术手段。
A method based on ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was established for the simultaneous determination of catecholamines(CAs) and their three metabolites in blood. This method requires only 100 µL of blood sample,which is purified using an ultrafiltration centrifuge tube and extracted by solid-phase extraction. Separation is achieved using an HSS PFP column,with acetonitrile-0.1% formic acid aqueous solution as the mobile phase for gradient elution. The samples were scanned by electrospray positive ion multiple reaction monitoring(MRM) mode and quantified by internal standard method. The results showed that the linearities of CAs and their metabolites were good in the concentration range of 0.5-50 ng/mL(
r
²
>
0.99). The limits of detection and quantification were 0.2 ng/mL and 0.5 ng/mL,respectively. The recoveries of six target analytes at spiked levels of 1,10 and 50 ng/mL ranged from 68.9%-101%,with matrix effects ranging from 86.2%-102%,and the relative standard deviations(RSDs) from 2.3%-10%. The established method can provide effective technical means for clinical diagnosis and the detection and identification of epinephrine poisoning cases.
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