Simultaneous determination of captopril and S-benzoyl captopril in human blood by capillary gas chromatography-mass selective detection (original) (raw)
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Determination of Captopril in Human Blood by an Enzyme-linked Immunosorbent Assay
Journal of Pharmacy and Pharmacology, 1996
An immunoassay for the quantitation of the angiotensin-converting enzyme inhibitor, captopril in human plasma is described. Antisera very specific for captopril were produced by immunization with captopril conjugated to bovine serum albumin or porcine thyroglobulin via the drug's thiol group. The antibodies were used to develop an enzyme-linked immunosorbent assay (ELISA) with a detection limit of 0.3 ng mL-1 and intra- and inter-assay coefficients of variation of 7 and 12%, respectively. Apart from stabilizing captopril by the addition of N-ethyl maleimide, the assay was used to detect the drug in human plasma without further extraction or purification. Our immunoassay provides a very sensitive and rapid (four hours) alternative for the study of captopril pharmacokinetics.
Biomedical Chromatography, 2001
Captopril, a well-known angiotensin converting enzyme (ACE) inhibitor, is widely used for treatment of arterial hypertension. Recent studies suggest that it may also act as a scavenger of free radicals because of its thiol group. Therefore, the present study describes a rapid, sensitive and relatively simple method for the detection of captopril in biological tissues with reversephase HPLC. Captopril was first derivatized with ThioGlo 2 3 [3H-Naphto[2,1-b]pyran,9-acetoxy-2-(4-(2,5-dihydro-2,5-dioxo-1Hpyrrol-1-yl)phenyl-3-oxo-)]. It was then detected by fluorescence-HPLC using an Astec C 18 column as the stationary phase and a water:acetonitrile:acetic acid:phosphoric acid mixture (50:50; 1 mL/L acids) as the mobile phase (excitation wavelength, 365 nm; emission wavelength, 445 nm). The calibration curve for captopril was linear over a range of 10-2500 nM and the coefficient of variation acquired for the within-and between-run precision for captopril was 0.5 and 3.8%, respectively. The detection limit of captopril with this method was found to be 200 fmol/20 mL injection volume. Its relative recovery from biological samples was determined to the range from 93.3 to 105.3%. Based on these results, we believe that our method is advantageous for captopril determination.
Talanta, 2009
A new simple, sensitive and selective liquid chromatography coupled with mass spectrometry (LC/MS) method for quantification of captopril after precolumn derivatization with p-bromo-phenacyl-bromide in human plasma was validated. Plasma samples were analysed on a monolithic column (Cromolith Performance-RP 18e, 100 mm × 4.6 mm I.D., 3 m) under isocratic conditions using a mobile phase of a 40:60 (v/v) mixture of acetonitrile and 0.1% (v/v) formic acid in water. The flow rate was 1 mL/min at the column temperature of 30 • C. In these chromatographic conditions, the retention time was 4.4 min for captopril derivative. The detection of the analyte was in MRM mode using an ion trap mass spectrometer with electrospray positive ionisation. The monitored ions were 216, 253, 255, 268, 270 m/z derived from 415 m/z for derivatized captopril. The sample preparation was very simple and consisted in plasma protein precipitation from 0.2 mL plasma using 0.3 mL methanol after the derivatization reaction was completed. Calibration curves were generated over the range of 10-3000 ng/mL with values for coefficient of correlation greater than 0.993 and by using a weighted (1/y 2 ) quadratic regression. The values for precision (CV %) and accuracy (relative error %) at quantification limit were less than 9.9% and 3.9%, for within-and between-run, respectively. The mean recovery of the analyte was 99%. Derivatized samples demonstrated good short-term, long-term, post-preparative and freeze-thaw stability. This is the first reported LC-MS/MS method for analysis of captopril in human plasma that uses protein precipitation as sample processing procedure. The method is very simple and allows obtaining a very good recovery of the analyte. The validated LC-MS/MS method has been applied to a pharmacokinetic study of 50 mg captopril tablets on healthy volunteers.
IJPSM, 2021
Captopril is the most commonly prescribed ACE-Inhibitor class of drugs because it is easily accessible and affordable. Therefore, to ensure drug quality, captopril levels were determined. This review article aims to provide an overview of the various analytical techniques that have been carried out in selecting the groups of captopril in both pharmaceutical dosage forms and biological matrices. Some of these analytical methods include the UV-Visible spectrophotometric method, high-performance liquid chromatography (HPLC), voltammetry, and flow injection. The data collection process in this review article is to collect research journals through trusted sites in the last ten years (2011-2021) with the search keywords "Determination of Captopril," "Analysis of Captopril on Pharmaceutical Preparations," and Analysis of Captopril on Biological Matrices." From the data that has been collected, the voltammetric method is the most widely used analytical technique in determining captopril for both pharmaceutical preparations and biological matrices in the last ten years.
Journal of Pharmaceutical and Biomedical Analysis, 1997
A rapid, simple and sensitive assay was developed for determination of captopril in human serum. We employed silica gel cartridge for efficient extraction of captopril adduct from human serum. Captopril was trapped with p-bromophenacyl bromide (pBPB) to give captopril-pBPB adduct. A 4-ml benzene extract of 1 ml acidified serum was passed through 1 ml silica gel cartridge. Potential interfering compounds were removed with 4-ml benzene wash. The captopril-pBPB adduct was eluted with 0.5 ml acetonitrile. Of this acetonitrile solution (100 ~tl) was injected on an ODS reverse phase HPLC column (chromatography conditions; mobile phase; acetonitrile water acetic acid (225:270:5, v/v/v), flow rate; 1 ml rain ~, detection; UV at 263 nm). It is found that this method is accurate and does not require time consuming evaporation-concentration steps. Recovery exceeds 94% and analytical responses are linear over captopril concentration range from 50 up to 1000 ng ml-i. The coefficients of variation from 108 ng ml t to 605 ng ml ~ ~ varied between 3.7-7.7% and the relative error did not exceed 3.7%. Therefore, this method can be used for routine clinical monitoring and in pharmacokinetic studies of captopril.
Current Analytical Chemistry, 2010
A sensitive and simple Gas Chromatographic-Mass Spectrometric method was developed and validated for the determination of captopril in human plasma. Thiosalicylic acid was used as an internal standard, and plasma extraction was performed by solid phase extraction. The limit of quantification was 0.5 ng/mL with signal to noise ratio greater than 5. The calibration curve was linear from 1 to 160 ng/mL with r(2) greater than 0.99. The coefficient of variation for within and between assay imprecision of the standards and for the limit of quantification were <= 10 % and <= 7 %, respectively. The percentage of inaccuracy for within-and between-assay including lower and upper limits of quantitation were < 8 % and <= 6 %, respectively. The absolute recovery of captopril and thiosalicylic acid in plasma were greater than 98 % and 99 %, respectively. The high sensitivity and accuracy of this method allowed us to measure low concentrations of captopril in plasma for bioequivalence ...
Separation methods for captopril in pharmaceuticals and biological fluids
Journal of Separation Science, 2012
(CAP) is an orally active angiotensin-converting enzyme (ACE) inhibitor and has been widely used for management of hypertension and congestive heart failure. CAP lacks an aromatic chromophore required for facile direct UV detection and also has two chiral centers. These factors can render the determination of CAP in complex matrices challenging. This review covers more than 20 years of analytical research on this drug, focusing mainly on pharmaceutical and biological applications. The primary separation techniques discussed are gas chromatography, liquid chromatography, and capillary electrophoresis. The structures of the CAP derivatizing agents as well as a table summarizing various HPLC methods are provided. A discussion of key recent chromatographic and electrophoretic methods for other ACE inhibitors is also present.
A simple reversed phase HPLC method have been successfully developed and validated for the quantitative determination of captopril (CAP) in bulk material, pharmaceutical formulation and serum. Purospher Start C 18 (250cm x 4.6mm, 5µm) and Hypersil ODS C18 (150×4.6mm, 5micron) columns were used. The mobile phase, (methanol-water 50:50(v/v) pH 3.0 adjusted by phosphoric acid), was delivered at a flow rate of 1mLmin -1 , eluent was monitored using UV detector at 215, 220, 225 nm. The proposed method is specific, accurate (99-102%), precise (intra-day variation 0.04-0.98 % and inter-day variation 0.06-1.5%) and linearity (R 2 >0.999) within the desired range 1.25-50 µgmL -1 concentration. The detection limit and quantification limit was 2.0 ngmL -1 and 8.0 ngmL -1 respectively. The anticipated method is applicable to routine analysis of CAP in pharmaceutical formulations as well as in human serum samples.