Satínský Dalibor, Neto Isabel, Solich Petr, Sklenákova Hana, Conceição M, Montenegro B S M, Araújo Alberto N
The Research Centre LN00B125, Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského, Hradec Králové, Czech Republic.
J Sep Sci. 2004 May;27(7-8):529-36. doi: 10.1002/jssc.200301644.
In this contribution, a new separation method for simultaneous determination of paracetamol, caffeine, acetylsalicylic acid, and internal standard benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith Flash RP-18e, 25-4.6mm column (Merck, Germany) and a FIAlab 3000 system (USA) with an 8-port selection valve and a 5 mL syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-(0.01 M) phosphate buffer (10:90, v/v) pH 4.05, flow rate 0.6 mL min(-1). UV detection was at 210 and 230 nm. The validation parameters showed good results: linearity (r >0.999) for all compounds, detection limits in the range 0.3-0.8 microg mL(-1), repeatability (RSD) of peak heights between runs in the range 1.10-4.30% at three concentration levels and intra-day repeatability of the retention times in the range 0.28-0.43%. The analysis time was <6 min. The method was found to be applicable for the routine analysis of the active compounds paracetamol, caffeine, and acetylsalicylic acid in pharmaceutical tablets.
在本论文中,基于一种新型的带有紫外检测的反相顺序注射色谱(SIC)技术,开发了一种同时测定对乙酰氨基酚、咖啡因、乙酰水杨酸和内标苯甲酸的新分离方法。在我们的研究中,使用了一根Chromolith Flash RP - 18e,25 - 4.6mm色谱柱(德国默克公司)以及一台配备8通进样阀和5 mL注射器的FIAlab 3000系统(美国)进行顺序注射色谱分离。所用流动相为乙腈 - (0.01 M)磷酸盐缓冲液(10:90,v/v),pH 4.05,流速0.6 mL min⁻¹。紫外检测波长为210和230 nm。验证参数显示结果良好:所有化合物的线性度(r > 0.999),检测限在0.3 - 0.8 μg mL⁻¹范围内,在三个浓度水平下,不同进样间峰高的重复性(RSD)在1.10 - 4.30%范围内,日内保留时间的重复性在0.28 - 0.43%范围内。分析时间小于6分钟。该方法被发现适用于药物片剂中活性成分对乙酰氨基酚、咖啡因和乙酰水杨酸的常规分析。