Yan Zhang, Li Ling, Liangjiao Qu, Wenyan Huang, Hongyan Zou
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引用次数: 0
摘要
医院急诊室因服用乌头品种不当导致乌头生物碱中毒,可导致恶性心律失常、心源性休克甚至死亡的报道屡见不鲜。本研究建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定人体血液和尿液中14种乌头生物碱的简便方法。血样和尿样采用支撑液萃取(SLE)纯化,UPLC-MS/MS分析。14种乌头生物碱在0.1 ~ 50 ng mL−1范围内呈良好的线性关系,相关系数大于0.999,检出限在0.002 ~ 0.019 ng mL−1之间。三种浓度水平下的平均加样回收率分别为80.0% ~ 110.1%和85.0% ~ 110.2%,相对偏差小于10%。血基质效应范围为88.3% ~ 109.8%,尿基质效应范围为91.4% ~ 103.6%。日内和日间的精确度均低于11%。最后,将该方法成功应用于临床中毒患者血、尿中乌头生物碱的测定,显示出其在临床急诊中毒诊断中的良好潜力。
Simultaneous Determination of 14 Aconitum Alkaloids in Blood and Urine by SLE-UPLC-MS/MS
Aconitum alkaloid poisoning which can lead to malignant arrhythmia, cardiogenic shock and even death has been frequently reported due to improper intake of Aconitum species in hospital emergency rooms. In this study, a simple method for simultaneous determination of 14 aconitum alkaloids in human blood and urine by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) was developed. Blood and urine samples were purified by supported liquid extraction (SLE) and analyzed by UPLC-MS/MS. Good linear relationships for 14 aconitum alkaloids were obtained in the corresponding range of 0.1–50 ng mL−1 with correlation coefficients greater than 0.999 and detection limits of between 0.002 and 0.019 ng mL−1. The average recoveries measured at three concentration levels ranged from 80.0% to 110.1% and 85.0% to 110.2% in spiked blood samples and urine samples, respectively, with the relative deviation less than 10%. The blood matrix effects ranged from 88.3% to 109.8%, while the urine matrix effects ranged between 91.4% and 103.6%. Both the intra-day and inter-day precisions were less than 11%. Finally, the method was successfully applied to the determination of aconitum alkaloids in the blood and urine of clinic poisoned patients showing its good potential for poison diagnosis in clinical emergency cases.
期刊介绍:
Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.