Development and Validation of a Headspace Gas Chromatographic Method for the Determination of Methyl Bromide Content in Itraconazole API

Babu, Mannem Durga; Kishore, Medikondu; Babu, K. Surendra

doi:10.18052/www.scipress.com/ilcpa.59.160

ILCPA

2015

DOI: 10.18052/www.scipress.com/ilcpa.59.160

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Development and Validation of a Headspace Gas Chromatographic Method for the Determination of Methyl Bromide Content in Itraconazole API

Mannem Durga Babu¹,

Medikondu Kishore²,

K. Surendra Babu³

Abstract: ABSTRACT. To provide quality control over the manufacture of any API, it is essential to develop highly selective analytical methods. Gas chromatography with headspace (HSGC) is widely used for the determination of residual impurities and solvents in API's. In the current article we are reporting the development and validation of a rapid and specific Head space gas chromatographic (HSGC) method for the determination of methyl bromide in Itraconazole API. The developed method was validated in terms of specifici… Show more

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Shorter and Rugged Analytical GC Method for Residual Solvents Content in Active Pharmaceutical Ingredient

Ramanjaneyulu

Rao²,

Shyamala

2021

Journal of Chromatographic Science

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This work describes the highly selective and sensitive robust analytical method (gas chromatography) for the qualitative and quantitative analysis of commonly used residual solvents (like methanol, ethanol, acetonitrile, dichloromethane, methyl tert-butyl ether, n-hexane, 1-propanol, ethyl acetate, tetrahydrofuran, N,N-diisopropylethylamine (DIPEA) and dimethylformamide), in an active pharmaceuticals ingredients. The developed method was optimized with good resolution (>1.9 between close eluting solvents) and a shorter run time (20 min). All the solvents were separated using GC column DB–624, 30-m length, 0.32-mm diameter, 1.8-μm particle size, nitrogen as a carrier gas and recorded the signals using flame ionization detector (FID). Further, analytical method validation has been performed for the developed analytical method and the validation results demonstrated its routine application for the determination of residual solvents content by GC–head space (HS). The practical application was demonstrated by the suitable API batch analysis (having sample Con. 40 mg/mL). The present developed method has more advantages than the other methods for the qualitative and quantitative applications, such as shorter runtime, selective for multiple solvents (11 organic solvents) analysis at a time, highly sensitive at ppm levels. This GC–HS method could be used for the qualitative and quantitative determination of the residual solvents content in APIs.

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Shorter and Rugged Analytical GC Method for Residual Solvents Content in Active Pharmaceutical Ingredient

Ramanjaneyulu

Rao²,

Shyamala

2021

Journal of Chromatographic Science

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Development and Validation of a Rapid and Sensitive LC-APCI-MS/MS Method for the determination of three N-nitrosamine impurities in Varenicline tartrate drug substance and drug products

Vidyamani,

Ramachandran,

Durga Babu

et al. 2024

RJPT

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Nitrosamines impurities may be present in low levels in a variety of products that people are exposed to every day. After thorough investigations, regulatory agencies have outlined that the formation of nitrosamines is possible in the presence of secondary, tertiary, or quaternary amines and nitrite salts under acidic reaction conditions. For safety purpose, all API manufacturers must be developed methods to monitor the low levels of each nitrosamine impurity before the release the individual batches. In this article, we have developed novel, rapid and sensitive liquid chromatography Atmospiric pressure chemical ionization Mass spectroscopy (LC-APCI-MS/MS) method for the determination of N-Nitroso Dimethylamine (NDMA), N-Nitroso Diethylamine (NDEA) and N-Nitroso varenicline impurities in the Varenicline Tartrate drug substance and Drug products. Chromatographic separation is achieved using Inert sustain AQ C18 150 × 4.6mm, 3.0μ column with 0.1% formic acid in water as mobile phase A and 0.1% formic acid in methanol as mobile phase B at the 0.6 mL/min flow rate by using gradient mode of elution upto the 25 minutes total run time. The three impurities are successfully ionized and quantified in positive mode of atmospheric pressure chemical ionization (APCI) using multiple reaction monitoring (MRM). This method was validated according to ICH Q2 (R1) guidelines. The method provided excellent S/N ratios with a high linearity range of 0.66-19.88 ppm with respect to Varenicline Tartrate sample concentrations with a regression coefficient >0.995. The recovery for the method was established with a protocol of three-step sample preparation and was satisfactory within 85-115%. The determined LOQ (0.66 ppm) and LOD (0.22 ppm) values are very low with respect to sample concentration which shows the sensitivity Performance of the method. The method can be routinely applied for the detection of N-nitrosamine impurities (NDMA, NDEA and N-Nitroso varenicline) in Varenicline Tartrate drug substance and Drug products.

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Development and Validation of a Headspace Gas Chromatographic Method for the Determination of Methyl Bromide Content in Itraconazole API

Cited by 2 publications

References 2 publications

Shorter and Rugged Analytical GC Method for Residual Solvents Content in Active Pharmaceutical Ingredient

Shorter and Rugged Analytical GC Method for Residual Solvents Content in Active Pharmaceutical Ingredient

Development and Validation of a Rapid and Sensitive LC-APCI-MS/MS Method for the determination of three N-nitrosamine impurities in Varenicline tartrate drug substance and drug products

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