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首页> 外文期刊>Journal of mass spectrometry: JMS >Simultaneous quantitation of nicorandil and its denitrated metabolite in plasma by LC-MS/MS: Application for a pharmacokinetic study
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Simultaneous quantitation of nicorandil and its denitrated metabolite in plasma by LC-MS/MS: Application for a pharmacokinetic study

机译：LC-MS / MS同时定量测定血浆中尼可地尔及其反硝化代谢产物：在药代动力学研究中的应用

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摘要

A liquid chromatography-electrospray ionization tandem mass spectrometry method was developed and validated for the simultaneous quantitation of nicorandil and its denitrated metabolite, N-(2-hydroxyethyl)-nicotinamide, in rat plasma. After a liquid-liquid extraction step, chromatographic separation was performed on a ShinPack C_(18) column with an isocratic mobile phase composed of methanol and 2 mM aqueous ammonium acetate containing 0.03% (v/v) formic acid (33:67 v/v). Procainamide was used as an internal standard (IS). Selected reaction monitoring was performed using the transitions m/z 212 → m/z 135, m/z 166 → m/z 106 and m/z 236 → m/z 163 to quantify nicorandil, its denitrated metabolite and IS, respectively. Calibration curves were constructed over the range of 5-15 000 ng.ml~(-1) for both nicorandil and its metabolite. The mean relative standard deviation (RSD%) values for the intra-run precision were 5.4% and 7.3% and for the inter-run precision were 8.5% and 7.3% for nicorandil and its metabolite, respectively. The mean accuracy values were 100% and 95% for nicorandil and its metabolite, respectively. No matrix effect was detected in the samples. The validated method was successfully applied to a pharmacokinetic study after per os administration of nicorandil in rats.
机译：建立了液相色谱-电喷雾串联质谱法，并用于大鼠血浆中尼可地尔及其反硝化代谢产物N-（2-羟乙基）-烟酰胺的同时定量。液-液萃取步骤后，在ShinPack C_（18）色谱柱上进行色谱分离，该柱具有等度流动相，该流动相由甲醇和2 mM含0.03％（v / v）甲酸的乙酸铵水溶液（33:67 v / v）。普鲁卡因酰胺用作内标（IS）。使用转换m / z 212→m / z 135，m / z 166→m / z 106和m / z 236→m / z 163进行选定的反应监测，以分别量化尼可地尔，其脱硝代谢产物和IS。尼可地尔及其代谢物的校准曲线在5-15 000 ng.ml〜（-1）范围内绘制。尼可地尔及其代谢产物的运行内精密度的平均相对标准偏差（RSD％）值分别为5.4％和7.3％，运行间精密度的分别为8.5％和7.3％。尼可地尔及其代谢物的平均准确度值分别为100％和95％。在样品中未检测到基质效应。经验证的方法已在大鼠中口服尼可地尔后成功地用于药代动力学研究。

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