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样品固相净化及高效液相色谱法测定强心药维那利酮的血药浓度

Solid Phase Clean-up and Determination of Vesnarinone in plasma by High Performance Liquid Chromatography

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【作者】 吴苏澄伍朝筼

【Author】 Wu Sucheng;Wu Chaoyuan School of Pharmacy

【机构】 华西医科大学药学院华西医科大学药学院 成都军区总医院药局

【摘要】 作者用反相高效液相色谱法测定狗血浆中维那利酮的浓度,以自制氧化铝柱先净化血样,净化回收率为86.5±2.77%。在ODS柱上以甲醇-醋酸(1mmol/L)(55:45)为流动相,271nm波长检测,用4-甲氧基哌喹酮为内标,血浆维那利酮最低检出浓度为0.5ng/ml(R/N,3:1),5~500ng/10μl范围内峰面积比与浓度线性关系良好(r=0.99998)。日内和日间精密度分别为1.56%和1.98%(CV),回收率为96.26±5.40%;并用本法测定了麻醉狗灌胃给药后的血药浓度,得到了满意的结果。

【Abstract】 Vesnarinone, a new positiveinotropic agent, was synthesized by Tomi-naga et al of the Otsuka PharmaceuticalCo. Ltd. Institute in 1982. Determinationof Vesnarinone plasma level in dogs byreversed-phase HPLC was developed andpresented in this paper.A plasma samplepreparation was carried out by solid phasecleaned-up through neutral aluminum co-lumn(10×1cm I. D.)eluting with methanol.The chromatography consisted of a slim-packCLC ODS column (150×6.0mm I.D.) withmethanol: 1 mmol/L HAc (55:45) as themobile phase at a flow rate of 0.8 ml/minSpectrophotometric detection was at 271 nm.and column temparature was at 25℃. Using3,4-dihydro-6-(4-(4-methoxybenzoyl)-1-piperazinyl)-2 (1H) quinolinone as an inter-nal standard. The cleaned-up procedure issimple, rapid and satisfactory. The detectionlimit of vesnarinone was 0.5 ng/ml (R/N,3:1). The calibration curve was liner (r=0.99998) in the concentration range of 5-500ng/10μl. Within-day and day-to-day preci-sions(CV%) were 1.56 and 1.98. The reco-veries obtained from cleaned-up and spikedplasma samples were up to 86.52±2.77%and 96.26±5.46%, respectively.

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