关键词: Forensic toxicology Qualitative and quantitative analysis Toxic alkaloids UPLC–MS/MS

Mesh : Humans Tandem Mass Spectrometry / methods Chromatography, Liquid Chromatography, High Pressure Liquid / methods Alkaloids

来  源:   DOI:10.1016/j.legalmed.2023.102267

Abstract:
Toxic alkaloids are typically found in herbal medicines and have strong pharmacological effects and a broad therapeutic spectrum. On the other hand, toxic alkaloids exert toxicological activities in vivo; as such they have a narrow therapeutic window and can induce poisoning due to incorrect dose or misuse. In this view, there is an urgent need to develop a rapid and sensitive assay to detect these toxic alkaloids. This study developed a method for determining five common toxic alkaloids in blood, including brucine, strychnine, aconitine, mesaconitine, and hypaconitine using ultra-high liquid chromatography-tandem quadrupole/linear ion trap mass spectrometry (QTRAP UPLC-MS/MS). The analytes in this investigation were extracted with ether and detected using multiple reaction monitoring (MRM)-information-dependent acquisition (IDA)-enhanced product ion (EPI) scanning modes. SKF525A served as the internal standard (IS). The approach demonstrated excellent linearity, with a correlation coefficient (R) > 0.9964, and satisfactory sensitivity, with the limit of detection (LOD) of 0.31 ∼ 3.26 ng/mL and a limit of quantification (LOQ) of 1.13 ∼ 11.52 ng/mL. The extraction recovery (ER) was 78.8 ∼ 116.2%, the matrix effect (ME) was -12.3 ∼ 21.2%, and the method accuracy was 0.8 ∼ 12.8%. In addition, the intra-day precision and the inter-day precision (RSD) were 0.7% ∼ 7.4% and 0.4% ∼ 13.5%, respectively. The developed approach is sensitive and efficient, and offer significant application prospect in clinical monitoring and forensic detection of poisoning.
摘要:
有毒生物碱通常存在于草药中,具有很强的药理作用和广泛的治疗范围。另一方面,有毒生物碱在体内发挥毒理学活性;因此,它们具有狭窄的治疗窗口,并且由于剂量不正确或误用而可能引起中毒。在这个观点中,迫切需要开发一种快速、灵敏的方法来检测这些有毒生物碱。本研究建立了血液中五种常见毒性生物碱的测定方法,包括马钱子碱,马钱子碱,乌头碱,新乌头碱,和次乌头碱使用超高液相色谱-串联四极杆/线性离子阱质谱(QTRAPUPLC-MS/MS)。本研究中的分析物用乙醚提取,并使用多反应监测(MRM)-信息依赖采集(IDA)-增强产物离子(EPI)扫描模式进行检测。SKF525A作为内标(IS)。该方法表现出良好的线性度,相关系数(R)>0.9964,灵敏度令人满意,检测限(LOD)为0.31~3.26ng/mL,定量限(LOQ)为1.13~11.52ng/mL。提取回收率(ER)为78.8~116.2%,基质效应(ME)为-12.3~21.2%,方法准确度为0.8~12.8%。此外,日内精度和日间精度(RSD)分别为0.7%~7.4%和0.4%~13.5%,分别。所开发的方法是敏感和有效的,在中毒的临床监测和法医检测中具有重要的应用前景。
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