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Monitoring strychnine and brucine in biochemical samples using direct injection micellar liquid chromatography

机译:使用直接注射胶束液相色谱法监测生化样品中的士丁碱和马钱子碱

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摘要

Nux-vomica is a tropical plant that contains two ergot alkaloids i.e. strychnine and brucine which have pharmaceutical and toxic properties. In some places, for example in India, Nux-vomica is used in ayurvedic preparations in homeopathic medicine. As both compounds are toxic monitoring is required. In this work a method for the chromatographic determination of strychnine and brucine in various herbal/ayurvedic sample preparations, homeopathic medicines, containing Nux-vomica, seeds of Nux-vomica as well as in spiked serum and real urine samples are described. The method involves a direct injection micellar liquid chromatography technique that was optimised under ICH guidelines. Optimum conditions are a mobile phase composed by 0.10 M SDS-pentanol 4% (v/v)-NaH2PO4 buffered at pH 3 with UV detection at 258 nm, flow rate of 1 mL min~(-1), and temperature 25 °C. Under these conditions strychnine and brucine were analyzed in 15 and 11 min, respectively. Validation studies using ICH guidelines were performed to show that the proposed method was linear (r~2 >0.9997), with LODs (0.18 and 0.09) and LOQs (0.69 and 0.35), for strycnine and brucine, respectively. Repeatability intra- and inter-day was below of 2.50. The developed method can be useful for analyzing strychnine and brucine for quality control and other related forensic and clinical cases.
机译:Nux-vomica是一种热带植物,含有两种麦角生物碱,即士的宁和马钱子碱,它们具有药物和毒性。在某些地方,例如印度,Nux-vomica用于顺势疗法药物的印度草药制剂。由于这两种化合物都是有毒的,因此需要进行监测。在这项工作中,描述了色谱法测定各种草药/阿育吠陀样品制剂,含有Nux-vomica的顺势疗法药物,Nux-vomica的种子以及加标的血清和真实尿液样品中士的宁和马钱子碱的方法。该方法涉及直接注射胶束液相色谱技术,该技术已在ICH准则下进行了优化。最佳条件是流动相由0.10 M SDS-戊醇4%(v / v)-NaH2PO4组成,在pH 3缓冲,在258 nm处有UV检测,流速为1 mL min〜(-1),温度为25°C 。在这些条件下,分别在15分钟和11分钟内分析了士的宁和马钱子碱。使用ICH指南进行的验证研究表明,所提出的方法是线性的(r〜2> 0.9997),对士的宁和芥子碱的LOD分别为(0.18和0.09)和LOQ(0.69和0.35)。日内和日间重复性低于2.50。所开发的方法可用于分析士的宁和马钱子碱,以进行质量控制以及其他相关的法医和临床病例。

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