Chmielewska Aleksandra, Konieczna Lucyna, Plenis Alina, Bieniecki Michał, Lamparczyk Henryk
Medical University of Gdańsk, Faculty of Pharmacy, Hallera 107, PL-80-416 Gdańsk, Poland.
Biomed Chromatogr. 2006 Jan;20(1):119-24. doi: 10.1002/bmc.537.
A reversed-phase high-performance liquid chromatographic method with electrochemical detection for the quantitative determination of diclofenac potassium in plasma was developed. Naproxen was used as the internal standard. The drug and internal standard were isolated from plasma by extraction with dichloromethane and 2 M hydrochloric acid. Chromatographic separation was performed on a C18 column with methanol-water (68:32, v/v) adjusted to pH 3.2 with phosphoric acid as mobile phase. The oxidation potential for detection was established by constructing a voltammogram for diclofenac. The quantification limit for diclofenac in plasma was 5 ng mL(-1). Linearity of the method was confirmed in the range 5-2000 ng mL(-1), correlation coefficient 0.9998. Within-day relative standard deviations (RSDs) ranged from 0.66 to 14.00% and between-day RSDs from 0.59 to 15.78%. The method was successfully applied for the determination of pharmacokinetic parameters after ingestion of a 50 mg dose of diclofenac. Studies were performed on 18 healthy volunteers of both sexes.
建立了一种采用电化学检测的反相高效液相色谱法，用于定量测定血浆中的双氯芬酸钾。以萘普生作为内标。通过用二氯甲烷和2 M盐酸萃取，从血浆中分离出药物和内标。在C18柱上进行色谱分离，以甲醇 - 水（68:32，v/v）为流动相，用磷酸调节至pH 3.2。通过构建双氯芬酸的伏安图确定检测的氧化电位。血浆中双氯芬酸的定量限为5 ng mL(-1)。该方法在5 - 2000 ng mL(-1)范围内的线性得到确认，相关系数为0.9998。日内相对标准偏差（RSD）范围为0.66%至14.00%，日间RSD范围为0.59%至15.78%。该方法成功应用于50 mg剂量双氯芬酸摄入后的药代动力学参数测定。对18名男女健康志愿者进行了研究。
