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采用高效液相色谱-紫外检测法和毛细管电泳-电导检测法同时测定药物制剂中的咖啡因、对乙酰氨基酚和布洛芬。

Simultaneous determination of caffeine, paracetamol, and ibuprofen in pharmaceutical formulations by high-performance liquid chromatography with UV detection and by capillary electrophoresis with conductivity detection.

作者信息

Cunha Rafael R, Chaves Sandro C, Ribeiro Michelle M A C, Torres Lívia M F C, Muñoz Rodrigo A A, Dos Santos Wallans T P, Richter Eduardo M

机构信息

Instituto de Química, Universidade Federal de Uberlândia, Av. João Naves de Ávila, 2121, Uberlândia, MG, Brazil.

Departamento de Química.

出版信息

J Sep Sci. 2015 May;38(10):1657-62. doi: 10.1002/jssc.201401387. Epub 2015 Apr 20.

Abstract

Paracetamol, caffeine and ibuprofen are found in over-the-counter pharmaceutical formulations. In this work, we propose two new methods for simultaneous determination of paracetamol, caffeine and ibuprofen in pharmaceutical formulations. One method is based on high-performance liquid chromatography with diode-array detection and the other on capillary electrophoresis with capacitively coupled contactless conductivity detection. The separation by high-performance liquid chromatography with diode-array detection was achieved on a C18 column (250×4.6 mm(2), 5 μm) with a gradient mobile phase comprising 20-100% acetonitrile in 40 mmol L(-1) phosphate buffer pH 7.0. The separation by capillary electrophoresis with capacitively coupled contactless conductivity detection was achieved on a fused-silica capillary (40 cm length, 50 μm i.d.) using 10 mmol L(-1) 3,4-dimethoxycinnamate and 10 mmol L(-1) β-alanine with pH adjustment to 10.4 with lithium hydroxide as background electrolyte. The determination of all three pharmaceuticals was carried out in 9.6 min by liquid chromatography and in 2.2 min by capillary electrophoresis. Detection limits for caffeine, paracetamol and ibuprofen were 4.4, 0.7, and 3.4 μmol L(-1) by liquid chromatography and 39, 32, and 49 μmol L(-1) by capillary electrophoresis, respectively. Recovery values for spiked samples were between 92-107% for both proposed methods.

摘要

对乙酰氨基酚、咖啡因和布洛芬存在于非处方药物制剂中。在本研究中,我们提出了两种同时测定药物制剂中对乙酰氨基酚、咖啡因和布洛芬的新方法。一种方法基于配有二极管阵列检测的高效液相色谱法,另一种基于配有电容耦合无接触电导检测的毛细管电泳法。采用配有二极管阵列检测的高效液相色谱法,在C18柱(250×4.6 mm(2),5μm)上进行分离,流动相为梯度洗脱,由40 mmol L(-1) pH 7.0的磷酸盐缓冲液中20 - 100%的乙腈组成。采用配有电容耦合无接触电导检测的毛细管电泳法,在熔融石英毛细管(长度40 cm,内径50μm)上进行分离,使用10 mmol L(-1) 3,4 - 二甲氧基肉桂酸酯和10 mmol L(-1) β - 丙氨酸,用氢氧化锂将pH调至10.4作为背景电解质。通过液相色谱法在9.6分钟内完成对所有三种药物的测定,通过毛细管电泳法在2.2分钟内完成。咖啡因、对乙酰氨基酚和布洛芬的液相色谱检测限分别为4.4、0.7和3.4 μmol L(-1),毛细管电泳检测限分别为39、32和49 μmol L(-1)。两种方法加标样品的回收率均在92 - 10

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