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首页> 外文期刊>Pharmaceutical Chemistry Journal >STRUCTURE OF CHEMICAL COMPOUNDS, METHODS OF ANALYSIS AND PROCESS CONTROL DETERMINING NIFERIDIL IN BLOOD SERUM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
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STRUCTURE OF CHEMICAL COMPOUNDS, METHODS OF ANALYSIS AND PROCESS CONTROL DETERMINING NIFERIDIL IN BLOOD SERUM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

机译：反相高效液相色谱法测定化学成分的化学化合物结构，分析方法及过程控制

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A reversed-phase high-performance liquid chromatography (RP-HPLC) technique is described that can be used for the determination of niferidil in rat blood serum. The RP-HPLC procedure is carried out on a Silasorb SF C_8 column (150 x 4 mm, 5 urn) eluted with a MeOH:H_2O (45:55) mobile phase (adjusted to pH 2.5 with orthophosphoric acid and then to pH 3.5 with propylamine) at a flow rate of 1 mL/min with UV detection at 265 nm. The procedure is as follows: mix rat blood serum (1 mL), NaHCO_3 solution (100 muL), and CHCl_3 (3 mL) in a 10-mL glass centrifuge tube. Shake for 2 min and centrifuge at 3,000 rpm for 10 min. Transfer the CHCl_3 phase into another tube and evaporate to dryness under a stream of nitrogen. Reconstitute the residue in mobile phase (100 muL) and inject an aliquot (20 muL) into the chromatographic column. The average recovery of niferidil is 70%. The detection limit is 0.01 mug/mL. The method was linear from 0.02 to 0.5 mug/mL with a correlation coefficient of 0.968. The coefficient of variation was less than 12% within a day (n = 5). The proposed method was successfully used to determine some pharmacokinetic parameters after intravenous injection of niferidil in rats.
机译：描述了一种反相高效液相色谱（RP-HPLC）技术，可用于测定大鼠血清中的niferidil。 RP-HPLC方法在Silasorb SF C_8色谱柱（150 x 4 mm，5 urn）上进行，用MeOH：H_2O（45:55）流动相洗脱（用正磷酸调节至pH 2.5，然后用5％的pH调节至pH 3.5）丙胺）以1 mL / min的流速通过265 nm的UV检测。步骤如下：在10 mL玻璃离心管中混合大鼠血清（1 mL），NaHCO_3溶液（100μL）和CHCl_3（3 mL）。摇动2分钟，然后以3,000 rpm离心10分钟。将CHCl_3相转移到另一个试管中，并在氮气流下蒸发至干。重新配制流动相中的残留物（100μL），并将等分试样（20μL）注入色谱柱。 Niferidil的平均回收率为70％。检出限为0.01杯/毫升。该方法在0.02至0.5马克杯/毫升之间呈线性，相关系数为0.968。一天之内变异系数小于12％（n = 5）。所建议的方法已成功用于确定大鼠静注尼非地尔后的一些药代动力学参数。

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