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用于多组分镇痛药测定的反相高效液相色谱法的优化。

Optimization of the RP-HPLC method for multicomponent analgetic drug determination.

作者信息

Ivanovic D, Medenica M, Malenovic A, Jancic B, Misljenovic Dj

机构信息

Department of Drug Analysis, Faculty of Pharmacy, Belgrade, Yugoslavia.

出版信息

Boll Chim Farm. 2003 Nov;142(9):386-9.

Abstract

The optimization of RP-HPLC method defined the simultaneous influence of some important conditions, such as the mobile phase composition, pH of the mobile phase and temperature, on the separation and determination. The RP-HPLC method was done for the determination of paracetamol, caffeine and propyphenazone in a multicomponent pharmaceutical dosage form. The separation factor values define the optimal conditions, which were confirmed by analysing the appropriate mathematical models. The chromatographic system Hewlett Packard 1100 consisted of a HP 1100 pump, HP 1100 UV-VIS detector and HP integrator. Separations were performed on a Beckman Ultrasphere ODS 4.6 x 150 mm, 5 microns particle size column. Samples were introduced through a Rheodyne injector valve with a 20 microL sample loop. UV detection was performed at 265 nm and phenobarottons was used as an internal standard. The optimization was performed within the pH range from 2.5 to 6.0; temperature range from 20 degrees C to 55 degrees C and composition of the mobile phase methanol-water from (30:70 V/V) to (65:35 V/V). The three-D graphs, constructed with sixty-four experimental points, confirmed the optimal conditions for the determination of the investigated analgetic drugs.

摘要

反相高效液相色谱(RP-HPLC)方法的优化确定了一些重要条件(如流动相组成、流动相pH值和温度)对分离和测定的同时影响。采用RP-HPLC法测定多组分药物剂型中的对乙酰氨基酚、咖啡因和异丙安替比林。分离因子值确定了最佳条件,通过分析适当的数学模型得到了证实。色谱系统为惠普1100,由惠普1100泵、惠普1100紫外可见检测器和惠普积分仪组成。在贝克曼超球ODS 4.6×150 mm、粒径5微米的色谱柱上进行分离。通过带有20微升进样环的Rheodyne进样阀进样。在265 nm处进行紫外检测,苯巴比妥用作内标。在pH值范围为2.5至6.0、温度范围为20℃至55℃以及流动相甲醇-水的组成范围为(30:70 V/V)至(65:35 V/V)内进行优化。用64个实验点构建的三维图证实了所研究的镇痛药测定的最佳条件。

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