The characterization of synthetic by-products byB/E linked scanning and high-resolution thermospray mass spectrometry

Dinallo, Roger M.; Davidson, Walter; Hansen, G.E.

doi:10.1002/bms.1200200506

Cited by 3 publications

(1 citation statement)

References 3 publications

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“…Three papers have been published on chromatographic methods that study different aspects of nevirapine. Dinallo et al [20] reported the characterization of synthetic byproducts by B/E linked scanning and high-resolution thermospray mass spectrometry. Cohen et al [21] and Palladino et al [22] separately reported the studies of the binding environment of nevirapine to reverse transcriptase of HIV-1 by high-performance liquid chromatography (HPLC) and photoaffinity crosslinking.…”

Section: Introductionmentioning

confidence: 99%

Stability indicating HPLCc method for impurities estimation of nevirapine in extended release tablet dose

Reddiaha¹,

Devib²,

Mukkantic³

et al. 2012

Annales UMCS Chemia

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A novel, sensitive and selective Reverse phase High performance liquid chromatographic method was developed for quantitative determination of Nevirapine in its Extended Tablet dosage forms. The synthetic non-nucleoside reverse transcriptase inhibitor analogues (NNRTI) Nevirapine form one of the Extended dosage in HIV. It belongs to a group of anti-HIV medicines called non-nucleoside reverse transcriptase inhibitors (NNRTIs). The method is applicable to the quantification of related compounds of Nevirapine forming one of the fixed Extended dosage. Chromatographic separation of Nevirapine from the possible impurities and the degradation products was achieved on an Supelcosil LC-ABZ 150 x 4.6 mm, 5.0 m column; Ammonium Orthophosphate pH 5.0 as mobile phase A and Acetonitrile taken as mobile phase B in the ratio (85 : 15). The flow rate was 1.0 mL/min, and the detection was done at 220 nm. The above developed HPLC method was further subjected to hydrolytic, oxidative, photolytic and thermal stress conditions. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, and ruggedness.

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Section: Introductionmentioning

confidence: 99%

Stability indicating HPLCc method for impurities estimation of nevirapine in extended release tablet dose

Reddiaha¹,

Devib²,

Mukkantic³

et al. 2012

Annales UMCS Chemia

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Improved thermospray accurate mass measurement using a magnetic sector instrument

Davidson

Dinallo

Hansen

1991

Biol. Mass Spectrom.

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A method permitting accurate mass measurement of full-scan thermospray mass spectra is presented. Improved resolution and sensitivity were achieved by the addition of source cryopumping. Ion beam stability was enhanced by adaptation of a vaporizer tip with a sapphire orifice. Large systematic errors, such as previously reported with currentcontrolled scanning and widely spaced reference ions, were greatly reduced by employing field-controlled magnetic scanning. The method permits measurements accurate to better than 10 ppm whie employing a simple polyethylene glycol standard.

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Validation of a High-Performance Liquid Chromatography Method for the Assay of and Determination of Related Organic Impurities in Nevirapine Drug Substance

Li¹,

Tougas²,

Cohen³

et al. 2000

Journal of Chromatographic Science

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Nevirapine (Viramune), a dipyridiodiazepinone, is a potent and highly specific nonnucleoside inhibitor of HIV-1 reverse transcriptase. This paper describes the validation of a specific, sensitive, and stability-indicating high-performance liquid chromatography method for the assay and determination of related organic impurities in nevirapine drug substance. This method uses a Supelcosil LC-ABZ column, a mobile phase of 20:80 (v/v) acetonitrile-25mM NH4H2PO4 (pH 5.0), and ultraviolet detection at a wavelength of 220 nm. This method was validated for specificity, linearity, accuracy, repeatability, detection limit, quantitation limit, stability of analyte solutions, robustness, and intermediate precision. Nevirapine is completely separated from all impurities. The method is shown to be linear with coefficients of determination r2 greater than 0.999. Average accuracy is 100.4% with a relative standard deviation of 0.7% for the assay. Accuracy ranges from 100.1 to 102.6% for related organic impurities. Repeatability is good, with relative standard deviations not more than 1.4%. The detection limit and the quantitation limit are determined to be 0.001 and 0.003%, respectively. Relative response factors of known organic impurities are determined, permitting the use of nevirapine at the 0.1% level as an external standard for the quantitation of these impurities. Analyte solutions are shown to be stable for at least 2 days at ambient temperature. The method is validated as robust, and intermediate precision is high. A system suitability test is developed and validated, and requirements are set.

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The characterization of synthetic by-products byB/E linked scanning and high-resolution thermospray mass spectrometry

Cited by 3 publications

References 3 publications

Stability indicating HPLCc method for impurities estimation of nevirapine in extended release tablet dose

Stability indicating HPLCc method for impurities estimation of nevirapine in extended release tablet dose

Improved thermospray accurate mass measurement using a magnetic sector instrument

Validation of a High-Performance Liquid Chromatography Method for the Assay of and Determination of Related Organic Impurities in Nevirapine Drug Substance

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