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Simultaneous evaluation of losartan and amlodipine besylate using second-derivative synchronous spectrofluorimetric technique and liquid chromatography with time-programmed fluorimetric detection

机译:二次导数同步荧光光谱法和液相色谱-程控荧光检测法同时评估氯沙坦和苯磺酸氨氯地平

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摘要

This study is concerned with two sensitive, fast and reproducible approaches; namely, second-derivative synchronous fluorimetry (method I) and reversed phase high-performance liquid chromatography with fluorimetric detection (method II) for synchronized evaluation of losartan (LOS) and amlodipine besylate (AML). Method I is based on measuring second-derivative synchronous fluorescence spectra of LOS and AML at Δλ = 80 nm in water. The experimental factors influencing the synchronous fluorescence of the considered compounds were sensibly adjusted. The chromatographic analysis was executed on a Nucleodur MN-C18 column of dimensions; 250 × 4.6 mm i.d. and 5 µm particle size). The fluorimetric detection was time-programmed at λem = 440 nm for AML (0.0–7.5 min) and at λem = 400 nm for LOS (7.5–10 min) after excitation at λex = 245 nm. The mobile phase is a blend of acetonitrile with 0.02 M phosphate buffer in a proportion of 45 : 55, pH 4.0, pumped using a flow rate of 1 ml min−1. The calibration plots were established to be 0.1–4.0 µg ml−1 for both drugs in method I and 0.05–4.0 µg ml−1 for both drugs in method II. The study was extended to the evaluation of the two drugs in their co-formulated tablets.
机译:这项研究涉及两种敏感,快速和可重复的方法。即二阶导数同步荧光法(方法I)和反相高效液相色谱-荧光检测法(方法II),用于氯沙坦(LOS)和苯磺酸氨氯地平(AML)的同步评估。方法I基于在水中测量Δλ= 80 nm时LOS和AML的二阶同步荧光光谱。合理调整了影响所考虑化合物同步荧光的实验因素。色谱分析在尺寸为Nucleodur MN-C18的色谱柱上进行; 250×4.6毫米内径和5 µm粒径)。在λex= 245 nm激发后,对于AML(0.0–7.5 min)在λem= 440 nm处进行荧光编程检测,对于LOS(7.5–10 min)在LOS(λe= 400 nm)进行时间编程。流动相是乙腈与0.02 M磷酸盐缓冲液的混合物,比例为45:55,pH 4.0,以1 ml min -1 的流速泵送。方法I中两种药物的标定图建立为0.1–4.0 µg ml -1 ,方法II中两种药物的标定图建立为0.05–4.0 µg ml -1 。该研究扩展到了两种药物在他们共同配制的片剂中的评价。

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