A Novel Validated GC-MS/MS Method for the Estimation of N-Nitroso Dimethyl Amine and N-Nitroso Diethyl Amine in Zidovudine.

IF 1.5 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of chromatographic science Pub Date : 2024-05-31 DOI:10.1093/chromsci/bmae008

Narayanareddy Papadasu, Ramakrishnareddy Kotanka, Raghuram Pannala

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引用次数: 0

Abstract

A novel method has been developed for the estimation of N-Nitroso dimethyl amine impurities (NDMA) and N-Nitroso diethyl amine (NDEA) in Zidovudine by using Gas chromatograph Triple Quadrupole Mass with Liquid autosampler (GC-MS/MS) and the method is validated as per International Conference on Harmonization recommendations. Sample analysis was executed for Zidovudine by developed method. Both NDMA and NDEA were detected in below quantitation limit for the Zidovudine batches. Efficient chromatographic separation was achieved on a DB-WAX 30 m length × 0.25 mm internal diameter, 0.5-μm film thickness, Triple quad-8040 GC-MS/MS. Quantification was carried out at Triple quad electron ionization source was at a column flow of 1.5 mL/min at a column oven temperature 50°C. The precision was in the range of 0.9-2.5% for NDMA and 0.8-2.3% for NDEA, and regression analysis shows as r value (correlation coefficient) of is >0.99. This method is capable to detect the NDMA and NDEA impurities in Zidovudine at a level of 0.006 ppm for limit of detection and 0.018 ppm for limit of quantitation with respect to test concentration of 66.66 mg/mL.

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估算齐多夫定中 N-亚硝基二甲基胺和 N-亚硝基二乙基胺的新型验证气相色谱-质谱/质谱法

本研究采用气相色谱仪-三重四极杆质谱-液体自动进样器（GC-MS/MS）建立了一种新型方法，用于估算齐多夫定中的 N-亚硝基二甲基胺杂质（NDMA）和 N-亚硝基二乙胺（NDEA），并根据国际协调会议的建议对该方法进行了验证。采用所开发的方法对齐多夫定进行了样品分析。在齐多夫定批次中检测到的 NDMA 和 NDEA 均低于定量限。在 DB-WAX 30 m 长×0.25 mm 内径、0.5-μm 薄膜厚度的 Triple quad-8040 GC-MS/MS 上实现了高效的色谱分离。定量在 Triple quad 电子电离源上进行，柱流量为 1.5 mL/min，柱温为 50°C。NDMA 的精密度为 0.9%-2.5%，NDEA 的精密度为 0.8%-2.3%，回归分析表明 r 值（相关系数）大于 0.99。该方法能够检测齐多夫定中的 NDMA 和 NDEA 杂质，以测试浓度 66.66 mg/mL 计，检出限为 0.006 ppm，定量限为 0.018 ppm。

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来源期刊

Journal of chromatographic science 化学-分析化学

CiteScore

2.90

自引率

7.70%

发文量

审稿时长

5.6 months

期刊介绍： The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.