A selective and sensitive UPLC–MS/MS approach for trace level quantification of four potential genotoxic impurities in zolmitriptan drug substance

Reddy, A. Vijaya Bhaskar; Venugopal, N.; Madhavi, G.; Reddy, K. Gangadhara; Madhavi, V.

doi:10.1016/j.jpba.2013.05.047

Cited by 32 publications

(17 citation statements)

References 15 publications

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“…The usefulness of this technique has been demonstrated for a wide range of applications in bioanalytical, environmental, and pharmaceutical research (Agnesod et al, 2013;Vijaya Bhaskar Reddy et al, 2013;Xiong et al, 2013). Thus, in the present work a highly rugged, selective and rapid UPLC-MS/MS method has been developed and fully validated as per the USFDA guidelines for simultaneous measurement of liensinine, isoliensinine and neferine in rat plasma using carbamazepine as internal standard (IS).…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of liensinine, isoliensinine and neferine in rat plasma by UPLC–MS/MS and application of the technique to pharmacokinetic studies

Dong

et al. 2015

Journal of Ethnopharmacology

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Section: Introductionmentioning

confidence: 99%

Simultaneous determination of liensinine, isoliensinine and neferine in rat plasma by UPLC–MS/MS and application of the technique to pharmacokinetic studies

Dong

et al. 2015

Journal of Ethnopharmacology

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“…In order to prove that the method is capable of its intended use, the newly developed method for the quantification of SHH and MAP PGIs in celecoxib drug substance was validated according to the international guidelines (Vijaya Bhaskar Reddy et al 2013;ICH 2005). …”

Section: Methods Validationmentioning

confidence: 99%

A selective and sensitive LC-MS/MS method for the simultaneous determination of twopotential genotoxic impurities in celecoxib

2014

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Background: Impurity profiling is now receiving critical attention from regulatory authorities. For trace level quantification of potential genotoxic impurities (PGIs), conventional analytical techniques like high-performance liquid chromatography (HPLC) and gas chromatography (GC) are inadequate; consequently, there is a great need to apply hyphenated analytical techniques to develop sensitive analytical methods for the analysis of pharmaceuticals. Methods: A selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of (4-sulfamoylphenyl)hydrazine hydrochloride (SHH) and (4-methyl-acetophenone)para-sulfonamide phenylhydrazine hydrochloride (MAP) PGIs in celecoxib active pharmaceutical ingredient (API). The LC-MS/MS analysis of SHH and MAP PGIs was done on Symmetry C18 (150 mm × 4.6 mm, 3.5 μm) analytical column, and the mobile phase used was 5.0 mM ammonium acetate-acetonitrile in the ratio of 30:70 (v/v). The flow rate used was 0.7 mL/min. Triple quadrupole mass detector coupled to positive electrospray ionization operated in multiple reaction monitoring (MRM) mode was used for the quantification of SHH and MAP PGIs. The method was validated as per International Conference on Harmonization (ICH) guidelines and was able to quantitate both SHH and MAP PGIs at 1.0 ppm with respect to 10 mg/mL of celecoxib. Results: The proposed method was specific, linear, accurate, precise, and robust. The calibration curves show good linearity between the concentration range of 0.06 and 7.5 ppm for both SHH and MAP PGIs. The correlation coefficient obtained was >0.9998 in each case. The method has very low limit of detection (LOD) and limit of quantification (LOQ). The obtained LOD and LOQ values were 0.02 and 0.06 ppm, respectively, for both SHH and MAP PGIs. For both the PGIs, excellent recoveries of 95.0% to 104.0% were obtained at a concentration range of 0.06 to 3.0 ppm. The developed method was also applied to determine the SHH and MAP PGIs in three formulation batches of celecoxib. Conclusions: The proposed method is simple and accurate and is a good quality control tool for the simultaneous quantitative determination of SHH and MAP PGIs at very low levels in celecoxib during its manufacturing.

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“…Some of the articles published in LC-MS/MS technique. [8][9][10] The literature survey related that some spectrometric methods were developed for the determination of pantoprazole sodium API. [11][12][13] A method has been reported for the determination of 2-chloromethyl-3,4-dimethoxy pyridine hydrochloride in pantoprazole API by RP-HPLC, GC-MS and LC/MS/MS.…”

Section: Introductionmentioning

confidence: 99%

A Selective and Sensitive Method Development and Validation by Lc–ms/MS Approach for Trace Level Quantification of Three Potential Genotoxic Impurities in Pantoprazole Sodium Drug Substance

2017

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A novel reverse-phase selective and sensitive liquid chromatography coupled with tandem mass spectrometric (LC-MS/MS) method was developed and validated for the trace analysis of N-(4-hydroxyphenyl) acetamide (GTI-A), N-(4-(difluoromethoxy) phenyl) acetamide (GTI-B) and 4-(difluoromethoxy)-2-nitroaniline (GTI-C) which are potential genotoxic impurities in pantoprazole drug substance. The optimized method utilizes a positive ion electrospray ionization in multiple reaction monitoring (MRM) detection modes with purosphere star RP 18 e (100 mm×4.6 mm, 3.0 µm) column. Solution-A was 0.1% formic acid in 1000 ml of water used as a buffer and solution-B was acetonitrile. The flow rate was 1.0 mL/min and gradient program was developed for rapid analysis and elution mode was monitored by a mass spectrophotometer. The method was validated as per International Conference on Harmonization (ICH) guidelines and the method capability for quantification was found to be 0.5 ppm with respect to sample concentration of 1mg/mL in pantoprazole sodium. The correlation coefficient obtained for all the three impurities was >0.9997 and the accuracy of the method was ranged between 96.3% and 104.3%.

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A selective and sensitive UPLC–MS/MS approach for trace level quantification of four potential genotoxic impurities in zolmitriptan drug substance

Cited by 32 publications

References 15 publications

Simultaneous determination of liensinine, isoliensinine and neferine in rat plasma by UPLC–MS/MS and application of the technique to pharmacokinetic studies

Simultaneous determination of liensinine, isoliensinine and neferine in rat plasma by UPLC–MS/MS and application of the technique to pharmacokinetic studies

A selective and sensitive LC-MS/MS method for the simultaneous determination of twopotential genotoxic impurities in celecoxib

A Selective and Sensitive Method Development and Validation by Lc–ms/MS Approach for Trace Level Quantification of Three Potential Genotoxic Impurities in Pantoprazole Sodium Drug Substance

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