Simultaneous quantification of atenolol and chlorthalidone in human plasma by ultra‐performance liquid chromatography–tandem mass spectrometry

Journal of Pharmaceutical Analysis

et al. 2017

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A sensitive and rapid liquid chromatography-tandem mass spectrometry (LC–MS/MS) method has been developed for the simultaneous determination of lisinopril (LIS) and hydrochlorothiazide (HCTZ) in human plasma using their labeled internal standards (ISs). Sample pre-treatment involved solid phase extraction on Waters Oasis HLB cartridges using 100 µL of plasma, followed by liquid chromatography on Hypersil Gold C18 (50 mm×3.0 mm, 5 µm) column. The analytes were eluted within 2.0 min using acetonitrile-5.0 mM ammonium formate, pH 4.5 (85:15, v/v) as the mobile phase. The analytes and ISs were analyzed in the negative ionization mode and quantified using multiple reaction monitoring. The method showed excellent linearity over the concentration range of 0.50–250.0 ng/mL for both the analytes. The intra-batch and inter-batch precision (% CV) was ≤5.26% and their extraction recoveries were in the range of 96.6%–103.1%. Matrix effect evaluated in terms of IS-normalized matrix factors ranged from 0.97 to 1.03 for both the analytes. The validated method was successfully applied to determine the plasma concentration of the drugs using 10 mg lisinopril and 12.5 mg hydrochlorothiazide fixed dose formulation in 18 healthy Indian volunteers.

“…The method was validated in accordance with the United States Food and Drug Administration (USFDA) guidance [35] and the procedures followed were similar to our previous method [36] .…”

Section: Resultsmentioning

confidence: 99%

Fast and sensitive LC–MS/MS method for the simultaneous determination of lisinopril and hydrochlorothiazide in human plasma

Journal of Pharmaceutical Analysis

et al. 2017

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“…Validation of the method was done for system suitability, selectivity, carryover, linearity, accuracy and precision, recovery, matrix effect, stability, dilution integrity and ruggedness as per the USFDA guidance [46] and was similar to that described in our previous work [47] . The detailed procedures are summarized in Supplementary material .…”

Section: Methodsmentioning

confidence: 99%

Application of an LC–MS/MS method for the analysis of amlodipine, valsartan and hydrochlorothiazide in polypill for a bioequivalence study

Parekh

Journal of Pharmaceutical Analysis

et al. 2017

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A sensitive and selective method has been proposed for the simultaneous determination of amlodipine (AML), valsartan (VAL) and hydrochlorothiazide (HCTZ) in human plasma by liquid chromatography–tandem mass spectrometry (LC–MS/MS). The analytes and their deuterated analogs were quantitatively extracted from 100 µL human plasma by solid phase extraction on Oasis HLB cartridges. The chromatographic separation of the analytes was achieved on a Chromolith RP18e (100 mm × 4.6 mm) analytical column within 2.5 min. The resolution factor between AML and VAL, AML and HCTZ, and VAL and HCTZ was 2.9, 1.5 and 1.4, respectively, under isocratic conditions. The method was validated over a dynamic concentration range of 0.02–20.0 ng/mL for AML, 5.00–10,000 ng/mL for VAL and 0.20–200 ng/mL for HCTZ. Ion-suppression/enhancement effects were investigated by post-column infusion technique. The mean IS-normalized matrix factors for AML, VAL and HCTZ were 0.992, 0.994 and 0.998, respectively. The intra-batch and inter-batch precision (% CV) across quality control levels was ≤ 5.56% and the recovery was in the range of 93.4%–99.6% for all the analytes. The method was successfully applied to a bioequivalence study of 5 mg AML + 160 mg VAL + 12.5 mg HCTZ tablet formulation (test and reference) in 18 healthy Indian males under fasting. The mean log-transformed ratios of Cmax, AUC0–120h and AUC0-inf and their 90% CIs were within 90.2%–102.1%. The assay reproducibility was demonstrated by reanalysis of 90 incurred samples.

“…Several analytical methods have been reported for the determination of ATOL in biological fluids and pharmaceutical formulations including voltammetry, potentiometry, gas chromatography–mass spectrometry, liquid chromatography‐mass spectrometry (LC–MS/MS), high‐performance liquid chromatography (HPLC), spectrophotometry, spectrofluorimetry, capillary electrophoresis and phosphorescence . Among the techniques presented above, however, spectrophotometry and capillary electrophoresis have some restrictions in selectivity and sensitivity.…”

Section: Introductionmentioning

confidence: 99%

Spectrofluorimetric determination of atenolol from human urine using high‐affinity molecularly imprinted solid‐phase extraction sorbent

2017

This study presents a novel, sensitive and selective molecularly imprinted solid-phase extraction (MISPE)-spectrofluorimetric method for the removal and determination of atenolol from human urine. Molecularly imprinted and non-imprinted polymers were synthesized thermally using a radical chain polymerization technique and used as solid-phase extraction sorbents. Acrylic acid ethylene glycol dimethacrylate, dibenzoyl peroxide and dichloroethane were used as a functional monomer, cross-linker, initiator and porogen, respectively. The calibration curve was in the range of 0.10-2.0 μg/ml for the developed method. Limit of detection and limit of quantification values were 0.032 and 0.099 μg/ml, respectively. Owing to the selectivity of the MISPE technique and the sensitivity of spectrofluorimetry, trace levels of atenolol have been successfully determined from both organic and aqueous media. Relatively high imprinting factor (4.18) and recovery results (74.5-75.3%) were obtained. In addition, intra- and interday precision values were 0.38-1.03% and 0.47-2.05%, respectively, proving the precision of the proposed method. Thus, a selective, sensitive and simple MISPE-spectrofluorimetric method has been developed and applied to the direct determination of atenolol from human urine.