Advanced LC-MS/MS method for selective quantification of nitrosamine impurities in Risperidone: Enhancing drug safety

IF 4.1 Q1 CHEMISTRY, ANALYTICAL

Talanta Open Pub Date : 2025-02-01 DOI:10.1016/j.talo.2025.100416

Hitesh Thumbar , Pankajkumar Nariya , Bhavin Dhaduk

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Abstract

In the current study, a simple, rapid, and sensitive analytical method was developed and validated for the determination and quantification of four nitrosamine drug substance-related impurities (NDSRIs) in Risperidone drug substance. Chromatographic separation was achieved on an ACE-5 PFP C18 column (150 mm × 4.6 mm × 3 µm) using gradient elution with 0.2 % formic acid and methanol. The method utilized a flow rate of 0.8 mL/min, an injection volume of 5 µL, and a column temperature of 40 °C. Positive electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode was used for quantification. The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.12 to 0.46 and 0.23–0.93 µg/mL, respectively. The calibration curves for NDIRs impurities (0.23–185.72 µg/mL) exhibited R² values between 0.998 and 0.999. Recoveries ranged varied from 94.9 to 124.4 %, with % RSD < 15.0 %. The results indicated that the method is reliable for monitoring all NINA, NBOP, NBP, and NB impurities in Risperidone.

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先进的LC-MS/MS方法选择性定量利培酮中亚硝胺类杂质：提高药物安全性

本研究建立了一种简便、快速、灵敏的利培酮原料药中4种亚硝胺类原料药相关杂质（NDSRIs）的测定和定量方法，并进行了验证。色谱分离采用ACE-5 PFP C18色谱柱（150 mm × 4.6 mm × 3µm），用0.2%甲酸和甲醇梯度洗脱。方法流速0.8 mL/min，进样量5µL，柱温40℃。采用多反应监测（MRM）模式下的正电喷雾电离（ESI）进行定量。检出限（LOD）为0.12 ~ 0.46，定量限（LOQ）为0.23 ~ 0.93µg/mL。NDIRs杂质（0.23 ~ 185.72µg/mL）的校准曲线R²值在0.998 ~ 0.999之间。回收率为94.9% ~ 124.4%，RSD为%；15.0%。结果表明，该方法可可靠地监测利培酮中所有的NINA、NBOP、NBP和NB杂质。

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