Analysis of diltiazem and its related substances by HPLC and HPLC/MS

Quaglia, M.G.; Donati, Enrica; Fanali, Salvatore; Bossù, E.; Montinaro, Annalisa; Buiarelli, Francesca

doi:10.1016/j.jpba.2004.11.050

Cited by 18 publications

(7 citation statements)

References 18 publications

(18 reference statements)

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“…Recently, HPLC–MS and CE methods have been reported to characterize the DTZ metabolites [19] , [20] , [21] , [22] . A RP-HPLC method using monolithic silica support for separation of DTZ and its impurities has been published [23] . Two validated stability indicating HPLC methods have also been reported for DTZ in bulk drug [24] and in tablets [25] .…”

Section: Introductionmentioning

confidence: 99%

Validated gradient stability indicating HPLC method for determining Diltiazem Hydrochloride and related substances in bulk drug and novel tablet formulation

Chatpalliwar¹,

Porwal²,

Upmanyu

2012

Journal of Pharmaceutical Analysis

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A stability-indicating liquid chromatographic method has been developed and validated for the determination of Diltiazem Hydrochloride (DTZ) together with its six related substances (Diltiazem sulphoxide, Imp-A, Imp-B, Imp-D, Imp-E, and Imp-F) in a laboratory mixture as well as in a novel tablet formulation developed in-house. Efficient chromatographic separation was achieved on a Hypersil BDS C18 (150 mm×4.6 mm, 5.0 μm) with mobile phase containing 0.2% Triethylamine (TEA) in gradient combination with acetonitrile (ACN) at a flow rate of 1.0 mL/min and the eluent was monitored at 240 nm. In the developed method, the resolution of DTZ from any pair of impurities was found to be greater than 2.0. The test solution and related substances were found to be stable in the diluent for 24 h. The developed method resolved the drug from its known impurities, stated above, and also from additional impurities generated when the formulation was subjected to forced degradation; the mass balance was found close to 99.9%.Regression analyses indicate correlation coefficient value greater than 0.997 for DTZ and its six known impurities. The LOD for DTZ and the known impurities was at a level below 0.02%. The method has shown good, consistent recoveries for DTZ (99.8–101.2%) and also for its six known impurities (97.2–101.3%). The method was found to be accurate, precise, linear, specific, sensitive, rugged, robust, and stability-indicating.

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Section: Introductionmentioning

confidence: 99%

Validated gradient stability indicating HPLC method for determining Diltiazem Hydrochloride and related substances in bulk drug and novel tablet formulation

Chatpalliwar¹,

Porwal²,

Upmanyu

2012

Journal of Pharmaceutical Analysis

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“…Optimal therapy with antiarrhythic drugs requires therapeutic drug monitoring (TDM) in order to avoid adverse effects and obtain the desired clinical benefit [9,10]. Many literatures have reported bioanalytical methods for antiarrhythic drugs determination, but the majority of these methods only focused on individual drugs mainly detected with HPLC-UV or LC-MS [11][12][13][14][15][16][17][18][19][20][21][22][23][24]. LC-MS/MS has proved to be an extremely important analytical technique that couples high sensitive and specific detection with high-resolution chromatographic separation.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of ten antiarrhythic drugs and a metabolite in human plasma by liquid chromatography—tandem mass spectrometry

Liu

Jia

et al. 2007

Journal of Chromatography B

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“…Although few methods for the determination of diltiazem in pharmaceutical matrixes have been reported, information on such metrological parameters is scarce [7–9, 11]. …”

Section: Introductionmentioning

confidence: 99%

Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

Sadeghi

Navidpour

Bayat

et al. 2013

Journal of Analytical Methods in Chemistry

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A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18 analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r 2 = 0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations.

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Analysis of diltiazem and its related substances by HPLC and HPLC/MS

Cited by 18 publications

References 18 publications

Validated gradient stability indicating HPLC method for determining Diltiazem Hydrochloride and related substances in bulk drug and novel tablet formulation

Validated gradient stability indicating HPLC method for determining Diltiazem Hydrochloride and related substances in bulk drug and novel tablet formulation

Simultaneous determination of ten antiarrhythic drugs and a metabolite in human plasma by liquid chromatography—tandem mass spectrometry

Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

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