Improved Ultra-Performance LC Determination of Indapamide in Human Plasma

Chromatographia (Impact Factor: 1.41). 09/2007; 66:119-122. DOI: 10.1365/s10337-007-0300-0


A simple, rapid, sensitive and selective method for the analysis of indapamide in human plasma, utilizing ultra performance
liquid chromatography (UPLC), has been developed and validated to satisfy FDA guidelines for bioanalytical methods. The analyte
and the internal standard, sulfamethazine, were isolated from plasma samples by liquid–liquid extraction with diethyl ether.
Separation was performed with an Acquity C18 column. The gradient composition of mobile phase was composed of acetonitrile
and sodium dihydrogenphosphate buffer (adjusted to pH 3.33 with 85% o-phosphoric acid) at a flow rate of 0.5mLmin−1. The assay exhibited a linear dynamic range of 1–100ngmL−1 for indapamide in human plasma. The limit of quantification (LOQ) was 1ngmL−1. The method was successfully applied to the pharmacokinetic and bioequivalence studies of indapamide formulations.

Download full-text


Available from: Selma Özilhan,
48 Reads
  • [Show abstract] [Hide abstract]
    ABSTRACT: Capillary electrophoresis with UV photo diode-array detection was utilized to adopt a new method for the assay of captopril and indapamide in pharmaceuticals and human plasma. Electrophoretic conditions controlling the analysis were optimized to develop separation, sensitivity and rapidity. The optimum conditions obtained were 100mM borate at pH 9.0, injection time 10.0s, voltage 25kV and column temperature 25°C with detection at 220nm. Relatively, wide dynamic ranges for captopril (1–100mgL−1) and indapamide (0.1–40mgL−1) were obtained. Also, the method recorded acceptable intra- and inter-day accuracy (89.8–97.9%) and precision (0.77–3.50%) in pharmaceutical formulations and human plasma. The sensitivity of the method was developed by the optimization and the preconcentration conducted for human plasma sample using liquid–liquid extraction. The limit of detection gained (0.075 and 0.045mgL−1 for captopril and indapamide, respectively) reached the level of both drugs possibly found in human plasma. The method is suitable to be applied in pharmaceutical industries for quality control and in clinical laboratories for therapeutic drug monitoring purposes.
    Chromatographia 01/2008; 68(5):437-442. DOI:10.1365/s10337-008-0707-2 · 1.41 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: Indapamide belongs to the class of thiazide-type diuretic drugs and is widely used in the treatment of hypertension and nephrolithiasis. In this work, a simple, rapid and efficient low density solvent (LDS) based ultrasound assisted emulsification microextraction (USAEME) method combined with high performance liquid chromatography-variable wavelength detection (HPLC-VWD) was investigated for the determination of a popular drug of abuse, indapamide, in human urine samples. The target compound was extracted from acidifed sample solution with a few microliter amount of LDS under USAEME method. The influence of several important experimental variables such as selection of the extraction solvent and its volume, ultrasonication time, pH and ionic strength were thoroughly examined and optimized. Under optimal conditions, calibration was linear in the concentration range from 1-100 ng mL-1 with a correlation coefficient of 0.9977 for the target analyte. The limit of detection based on signal to noise ratio of 3 was 0.3 ng mL-1 and the relative standard deviations varied from 1.2-6.6%. The proposed method provides a rapid, sensitive, low cost, easy to handle, and convenient procedure to determine indapamide in human urine samples.
    Analytical methods 03/2013; 5(10). DOI:10.1039/C3AY40187A · 1.82 Impact Factor