Determination of dimethyl sulfate genotoxic impurity in pantoprazole sodium sesquihydrate by derivatization method and UPLC/MS

IF 1.6 3区化学 Q3 PHYSICS, ATOMIC, MOLECULAR & CHEMICAL

International Journal of Mass Spectrometry Pub Date : 2024-09-14 DOI:10.1016/j.ijms.2024.117330

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Abstract

In this study, a new method has been developed and, the method has been validated to analyze dimethyl sulfate (DMS) which known as a genotoxic impurity. DMS has been detected in trace levels within the drug substance pantoprazole sodium sesquihydrate using the derivatization method. Triethylamine has been used as derivatization reagent. Due to the highly polar nature of the derivatization product, which is a quaternary ammonium ion, a polar retention Hilic column has been used for chromatographic separation. The Waters QDA detector has been used in the single ion recording (SIR) mode at m/z 116 for the detection of the quaternary ammonium ion. In this study, the recovery rates have been achieved within the range of 96.46–105.98%. The LOD has been determined as 1.94E-07 mg/mL, and the LOQ has been determined as 6.46E-07 mg/mL. From the results, it can be said that the improved method in this study, would enables fast and reliable solutions for routine quality control analyses for DMS in API companies that especially is producing PSS.

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利用衍生化方法和 UPLC/MS 测定倍半水合泮托拉唑钠中的硫酸二甲酯基因毒性杂质

本研究开发了一种新方法，并对该方法进行了验证，以分析被称为基因毒性杂质的硫酸二甲酯（DMS）。使用衍生化方法检测了药物泮托拉唑钠倍半水合物中的痕量 DMS。三乙胺被用作衍生试剂。由于衍生产物（季铵离子）具有高极性，因此使用了极性保留 Hilic 色谱柱进行色谱分离。沃特斯 QDA 检测器采用单离子记录（SIR）模式，在 m/z 116 处检测季铵离子。本研究的回收率在 96.46-105.98% 之间。LOD 为 1.94E-07 mg/mL，LOQ 为 6.46E-07 mg/mL。从结果来看，本研究中改进的方法可以为生产 PSS 的原料药公司的 DMS 常规质量控制分析提供快速可靠的解决方案。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

International Journal of Mass Spectrometry 物理-光谱学

CiteScore

3.60

自引率

5.60%

发文量

145

审稿时长

71 days

期刊介绍： The journal invites papers that advance the field of mass spectrometry by exploring fundamental aspects of ion processes using both the experimental and theoretical approaches, developing new instrumentation and experimental strategies for chemical analysis using mass spectrometry, developing new computational strategies for data interpretation and integration, reporting new applications of mass spectrometry and hyphenated techniques in biology, chemistry, geology, and physics. Papers, in which standard mass spectrometry techniques are used for analysis will not be considered. IJMS publishes full-length articles, short communications, reviews, and feature articles including young scientist features.