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建立和确证了适用于测定人血浆中尼美舒利含量的液相色谱-质谱(LC-MS)方法,并对尼美舒利参比和受试制剂进行生物等效性评价。人血浆样品(100μL)采用液液萃取法提取,内标为氢氯噻嗪。采用C_(18)柱,以甲醇-水(86:14,v/v)为流动相,选择离子监测负离子模式检测,尼美舒利m/z为307.00,内标氢氯噻嗪m/z为295.90。分析时间4.2分钟。尼美舒利在20.0-7000.0ng/mL浓度范围内线性关系良好,定量下限20.0ng/mL。内源性物质不干扰尼美舒利和内标的检测,无基质效应。尼美舒利和内标氢氯噻嗪的平均提取回收率均大于84.4%。所建立的方法已成功应用于尼美舒利生物等效性研究。
A liquid chromatography-mass spectrometry (LC-MS) method suitable for the determination of nimesulide in human plasma was established and validated, and the bioequivalence of nimesulide reference and test preparations was evaluated. Human plasma samples (100 μL) were extracted by liquid-liquid extraction and the internal standard was hydrochlorothiazide. The C 18 column with methanol-water (86:14, v / v) as the mobile phase was selected as the ion monitoring mode for negative ion detection. The m / z of nimesulide was 307.00 and the hydrochlorothiazide m / z was 295.90. Analysis time 4.2 minutes. Nimesulide showed a good linearity in the concentration range of 20.0-7000.0 ng / mL with a lower limit of quantitation of 20.0 ng / mL. Endogenous substances do not interfere with the detection of nimesulide and internal standard, no matrix effect. The average recoveries of nimesulide and internal standard hydrochlorothiazide were all above 84.4%. The established method has been successfully applied to nimesulide bioequivalence studies.