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RP-HPLC测定血浆中双氯芬酸钠的研究

A STUDY OF DETERMINATION OF DICLOFENAC SODIUM IN SERUM BY RP-HPLC

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【作者】 孙时良何怀冰刘德林文明王隆晏

【Author】 Sun Shiliang, He Huaibing, Liu Delin, Wen Ming, Wang Longyan (Instrumental Analysis Center, Shanghai Medical University, Shanghai)

【机构】 上海医科大学仪器分析中心实验室上海医科大学药学院上海医科大学药学院 1988届药学专业毕业生1988届药学专业毕业生

【摘要】 本文利用反相高效液相色谱法(RP-HPLC)对双氯芬酸钠(DS)血浓度的测定进行了研究,建立了灵敏、精确、简便、重现性好的分析方法。适用于药代动力学的研究。条件是在0.2mol/L NaAc-HAc缓冲溶液(pH5.0)中以乙醚-二氯甲烷3:1(V/V)提取。固定相为YWG C18H37,流动相为MeOH-0.02mol/L HAc(pH 5.5)65:35(V/V)、卡马西平(CZ)作内标,UV 280nm检测。线性范围0.24~22.8μg/ml,γ=0.999 9。最低检测浓度为60ng/ml。提取回收率为95.83%~97.58%。方法回收率为100.33%~106.46%。天内及天间精密度(GV)各为0.55%~1.11%及1.40%~2.91%。

【Abstract】 A simple, sensitive and reproducible RP-HPLC method was developed for the determiantion of diclofenac sodium (DS) in plasma. The samples were extracted by ether-dichloromethane in a pH5.0 HWc-NaAc buffer solution. A Gilson HPLC instrument, fitted with a YWG C8H17 10μm column (150×4.6mm) and a variable wavelength UV detector adjusted to 280nm, was used. The mobile phase contained of a mixture of MeOH and 0.02mol/L HAc 65:35(F/F). The flow rate was 1.0ml/min. Carbamazipine (CZ) was used as an internal standard. A linear calibration curve for DS was measured within a range of 0.24μg 22.8μg/ml. The limit of detection was 3.6ng and the lower concentration for detection was 60ng/ ml. Good coefficient of correlation (Y=-33.75+792.24X, r =0.999 9) was obtained, and an the average CV% of within and betwean-days were 0.88% and 2.35% respectively (n= 5). The anti-inflammatory agents for the routine analysis of large numbers of plasma samples usually obtained in pharmacokinetic studies were suitable.

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