Trace-level quantification of NDMA in levosulpuride active pharmaceutical ingredient and tablet formulation Using UFLC-MS/MS

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open Pub Date : 2024-11-03 DOI:10.1016/j.talo.2024.100375

Hemanth Vikram P․R , Gunjan Kumar , Rajashree Deka , Umme Hani , Nazima Haider , Sirajunisa Talath , Adil Farooq Wali , Dilipkumar Reddy Kandula , Narasimha M. Beeraka , Sinchana B Gopalaiah , Devi Sri Chiriki , Namitha Bannimath , Pramod Kumar , Bannimath Gurupadayya

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Abstract

Nitrosamine impurities identified in several pharmaceuticals during recent times has raised concerns leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated a ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of NDMA in Levosulpuride drug substance and tablet formulation. Current method utilizes a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Gemini NX-C18 column (150 × 4.6 mm, 3 µm) maintained at 40 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (methanol), with a total run time of 18 minutes. Current method achieved excellent linearity, recovery, precision, and sensitivity. Greenness of the developed method was evaluated using the GAPI, AGREE, and AES metrics. Current method is sensitive and selective for NDMA in levosulpuride drug substance and tablet formulations and can be employed for routine quality control analysis in pharmaceutical industry.

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使用 UFLC-MS/MS 在左旋舒必利活性药物成分和片剂中痕量定量 NDMA

近来，在一些药品中发现的亚硝胺杂质引起了人们的关注，导致了全球范围内的产品召回，因此有必要采用灵敏的液相和气相色谱法对亚硝胺杂质进行痕量检测。本研究开发并验证了一种超快速液相色谱-串联质谱（UFLC-MS/MS）方法，用于定量检测左旋舒必利（Levosulpuride）药物和片剂中的 NDMA。该方法采用三重四极杆分析仪、常压化学电离（APCI）电离源和多反应监测（MRM）扫描模式进行分析。色谱分离采用 Gemini NX-C18 色谱柱（150 × 4.6 毫米，3 微米），色谱柱温度保持在 40 °C。流动相包括溶剂 A（0.1% 甲酸水溶液）和溶剂 B（甲醇）的二元梯度，总运行时间为 18 分钟。该方法在线性、回收率、精密度和灵敏度方面均表现优异。使用 GAPI、AGREE 和 AES 指标对所开发方法的绿色性进行了评估。本方法对左旋舒必利药物和片剂中的 NDMA 具有良好的灵敏度和选择性，可用于制药行业的常规质量控制分析。

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