Development of an Efficient Method to Quantitatively Estimate Dichloroacetic Acid Genotoxic Impurity in Cetirizine Dihydrochloride by Liquid Chromatography–Mass Spectrophotometry

IF 1.7 4区医学 Q4 BIOCHEMICAL RESEARCH METHODS

Biomedical Chromatography Pub Date : 2025-08-07 DOI:10.1002/bmc.70189

Mithun M. Gharat, Pallavi T. Roy, Amit N. Gosar, Tabrez A. Shaikh, Gurumeet C. Wadhava, Nitin A. Mirgane

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Abstract

An LC–MS (liquid chromatography–mass spectrometry) methodology is developed for the precise analysis of dichloroacetic acid (DCAA) genotoxic impurity with high sensitivity and selectivity in a Cetirizine dihydrochloride (CTZ) drug substance. In accordance with the “threshold of toxicological concern (TTC),” the carryover of DCAA in a CTZ is done at a limit of 25 ppm in the sample. The present methodology is validated as per “International Council for Harmonization (ICH)” guidelines, and the detection limit and the quantitation limit are 0.4 and 1.2 ppm, respectively. The linearity study was conducted, and the coefficient of regression was found to be 0.9946. The method's accuracy was confirmed by the finding the percentage of recovered spiked DCAA in the drug, which ranged from 93.47% to 99.80%. Results indicated that the methodology was reliable, precise, and reproducible. The method can be extended for the determination of DCAA genotoxic impurity in a CTZ drug substance (API) samples by LC–MS.

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液相色谱-质谱法定量测定盐酸西替利嗪中二氯乙酸基因毒性杂质的方法研究。

建立了一种高效液相色谱-质谱联用方法，对盐酸西替利嗪（CTZ）原料药中二氯乙酸（DCAA）基因毒性杂质进行高灵敏度、高选择性的精确分析。根据“毒理学关注阈值（TTC）”，DCAA在CTZ中的残留在样品中的限制为25ppm。本方法根据“国际协调理事会（ICH）”指南进行验证，检测限和定量限分别为0.4和1.2 ppm。进行线性研究，回归系数为0.9946。结果表明，该方法的准确度在93.47% ~ 99.80%之间。结果表明，该方法可靠、精密度高、重复性好。该方法可推广应用于CTZ原料药（API）样品中DCAA基因毒性杂质的LC-MS测定。

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来源期刊

Biomedical Chromatography 生物-分析化学

CiteScore

3.60

自引率

5.60%

发文量

268

审稿时长

2.3 months

期刊介绍： Biomedical Chromatography is devoted to the publication of original papers on the applications of chromatography and allied techniques in the biological and medical sciences. Research papers and review articles cover the methods and techniques relevant to the separation, identification and determination of substances in biochemistry, biotechnology, molecular biology, cell biology, clinical chemistry, pharmacology and related disciplines. These include the analysis of body fluids, cells and tissues, purification of biologically important compounds, pharmaco-kinetics and sequencing methods using HPLC, GC, HPLC-MS, TLC, paper chromatography, affinity chromatography, gel filtration, electrophoresis and related techniques.