Structural elucidation of process-related impurities in escitalopram by LC/ESI-MS and NMR

Raman, Bhanu; Sharma, Brajesh; Ghugare, Pradeep D.; Nandavadekar, Sanjay; Singh, Dalbir; Karmuse, Pravin K.; Kumar, Ashok

doi:10.1016/j.jpba.2010.06.019

Cited by 16 publications

(13 citation statements)

References 12 publications

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“…Two different C18 columns were evaluated, but only on Zorbax Eclipse XDB were all the investigated compounds separated with the good peak shapes and minimum tailing. Earlier scientific papers have focused mostly on isolation, separation, and structure elucidation of citalopram and its impurities (22)(23)(24)(25)(26). Pharmacopoeias describing the official assays (27,28) have focused mostly on the different buffers used in mobile phases and on different ratios of acetonitrile and methanol as organic modifiers.…”

Section: Optimization Of Experimental Conditionsmentioning

confidence: 99%

“…Isolation, characterization, and structure elucidation of the degradation products of citalopram and the process-related impurities were performed using LC/electrospray ionization (ESI)-MS (22,23), and the hyphenated techniques LC/MS/MS, NMR spectroscopy, and FTIR spectroscopy (24)(25)(26). The United States Pharmacopeia (USP) 34 and the European Pharmacopoeia (EP) Ed.…”

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confidence: 99%

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Development and Optimization of an HPLC Analysis of Citalopram and Its Four Nonchiral Impurities Using Experimental Design Methodology

Tadić

Nikolić

Agbaba

2012

Journal of AOAC INTERNATIONAL

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In this study, the RP-HPLC method was investigated for the separation of citalopram and its four impurities by use of statistical experimental design. Initially, the influence of different experimental conditions (buffer pH, flow rate, and column temperature) on the chromatographic behavior of citalopram and its four impurities was investigated by use of partial least squares regression (PLSR) and multilayer perceptron (MLP) artificial neural networks (ANNs) trained by back-propagation. The developed models and the corresponding response surface plots were used to select the optimal HPLC conditions, buffer pH 7.0, flow rate 1.0 mL/ min, and column temperature 25 degrees C, for an efficient separation of citalopram and its four impurities. The elaborated HPLC method was found to be linear, specific, sensitive, precise, accurate, and robust. Retention times of citalopram and its impurities, obtained with the developed HPLC method, and the computed molecular parameters of the examined compounds were used in a quantitative structure retention relationship (QSRR) study. The PLSR and ANN algorithms were applied for the development of the QSRR methods. The MLP-two layers-ANN-QSRR model with root mean square error of prediction 0.105 and r(2) (observed versus predicted) 0.978 was selected. Since many different reaction conditions are applied for the synthesis of citalopram, different impurities and degradation products can be formed. Therefore, the developed QSRR model can be extended to the prediction of the retention times with the other citalopram impurities, degradation products, and metabolites.

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Section: Optimization Of Experimental Conditionsmentioning

confidence: 99%

mentioning

confidence: 99%

Development and Optimization of an HPLC Analysis of Citalopram and Its Four Nonchiral Impurities Using Experimental Design Methodology

Tadić

Nikolić

Agbaba

2012

Journal of AOAC INTERNATIONAL

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“…It is also an orally administered selective serotonin reuptake inhibitor (SSRI) prescribed for depression, panic, premenstrual dysphoric, and obsessivecompulsive disorder [15,16]. Methods such as chromatographic, spectrophotometric, colorimetric, and extractive colorimetric estimation using bromocresol green and methyl orange have been used in pharmaceutical and biological matrices [17][18][19][20].…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Tropaeolin 000-1 as a Colorimetric Reagent for Assay of Duloxetine and Escitalopram in Solid Dosage Form

Ganesh¹,

Aziz²,

Peng³

et al. 2016

Trop. J. Pharm Res

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“…Literature survey reveals several spectroscopic [2-4], HPLC [5,6] and HPTLC [7][8][9][10][11][12][13][14][15] methods for estimation of Escitalopram oxalate individually as well as combination with other drugs.…”

Section: Introduction Escitalopram Oxalate (Esc) Is the (Figure 1) Sementioning

confidence: 99%

Determination of Escitalopram Oxalate in Pharmaceutical Formulation by High Performance Liquid Chromatography

Charde¹,

Bhavsar²,

Chakole³

2012

Int J Pharmceut Chem

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ABSTRACT:A simple, precise and sensitive reverse-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitation of Escitalopram oxalate in pharmaceutical formulations. Chromatographic separation was achieved on a 250 × 4.6 mm, 5µ, C 18 column. The flow rate was 1ml/min and eluent was monitored by absorbance at 240 nm using a mixture of Acetonitrile and Buffer (pH 4.0) in the ratio of 25:75 (v/v). The retention times of Escitalopram oxalate was found to be 3.2 min. Calibration plots were linear in the concentration range of 2.5-80 µg mL -1 for Escitalopram oxalate. The total run time is 10 min. The proposed method was validated by testing its linearity, recovery, specificity, system suitability, precision (Interday and intraday), robustness and LOD/LOQ values and it was successfully employed for the determination of Escitalopram oxalate in pharmaceutical tablet formulations.

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Structural elucidation of process-related impurities in escitalopram by LC/ESI-MS and NMR

Cited by 16 publications

References 12 publications

Development and Optimization of an HPLC Analysis of Citalopram and Its Four Nonchiral Impurities Using Experimental Design Methodology

Development and Optimization of an HPLC Analysis of Citalopram and Its Four Nonchiral Impurities Using Experimental Design Methodology

Evaluation of Tropaeolin 000-1 as a Colorimetric Reagent for Assay of Duloxetine and Escitalopram in Solid Dosage Form

Determination of Escitalopram Oxalate in Pharmaceutical Formulation by High Performance Liquid Chromatography

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