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Cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE) for determination of Eszopiclone (Z-drug) using UV–Visible, HPLC and mass spectroscopic (MS) techniques: Spiked and in vivo analysis
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-01-06 , DOI: 10.1016/j.jchromb.2018.01.005
Shivpoojan Kori , Ankush Parmar , Jony Goyal , Shweta Sharma

A procedure for the determination of Eszopiclone (ESZ) from complex matrices i.e. in vitro (spiked matrices), as well as in vivo (mice model) was developed using cloud point extraction coupled with microwave-assisted back-extraction (CPE-MABE). Analytical measurements have been carried using UV–Visible, HPLC and MS techniques. The proposed method has been validated according to ICH guidelines and legitimate reproducible and reliability of protocol is assessed through intraday and inter-day precision < 3.61% and < 4.70%, respectively. Limit of detection has been obtained as 0.083 μg/mL and 0.472 μg/mL respectively, for HPLC and UV–Visible techniques, corresponding to assessed linearity range. The coaservate phase in CPE was back extracted under microwaves exposure, with isooctane at pre-concentration factor ~ 50 when 5 mL of sample solution was pre-concentrated to 0.1 mL. Under optimized conditions i.e. Aqueous-Triton X-114 4% (w/v), pH 4.0, NaCl 4% (w/v) and equilibrium temperature of 45 °C for 20 min, average extraction recovery has been obtained between 89.8 and 99.2% and 84.0–99.2% from UV–Visible and HPLC analysis, respectively. The method has been successfully applied to the pharmacokinetic estimation (post intraperitoneal administration) of ESZ in mice. MS analysis precisely depicted the presence of active N‑desmethyl zopiclone in impales as well as in mice plasma.



中文翻译:

浊点萃取与微波辅助反萃取(CPE-MABE)结合使用紫外可见,HPLC和质谱(MS)技术测定大黄酮(Z-药物):尖峰分析和体内分析

使用浊点萃取结合微波辅助反萃取(CPE-MABE),开发了一种从复杂基质中测定Eszopiclone(ESZ)的方法,即体外(加标基质)以及体内(小鼠模型)。使用UV-Visible,HPLC和MS技术进行了分析测量。所提出的方法已根据ICH指南进行了验证,并且合法的可重复性和协议的可靠性通过日内和日间精度分别<3.61%和<4.70%进行评估。HPLC和UV-Visible技术的检出限分别为0.083μg/ mL和0.472μg/ mL,对应于评估的线性范围。CPE中的共保守相在微波照射下反萃取,当将5 mL样品溶液预浓缩至0.1 mL时,用异辛烷的预浓缩因子〜50。在优化的条件下,即Triton X-114 4%(w / v),pH 4.0,NaCl 4%(w / v)和平衡温度为45°C的条件下进行20分钟,平均提取回收率在89.8和99.2之间分别来自UV-Visible和HPLC分析的%和84.0–99.2%。该方法已成功应用于小鼠ESZ的药代动力学估算(腹膜内给药)。MS分析精确描述了活性成分的存在 该方法已成功应用于小鼠ESZ的药代动力学估算(腹膜内给药)。MS分析精确描述了活性成分的存在 该方法已成功应用于小鼠ESZ的药代动力学估算(腹膜内给药)。MS分析精确描述了活性成分的存在N-去甲基佐匹克隆在黑斑病以及小鼠血浆中。

更新日期:2018-01-06
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