数字农科院2.0

Avoiding false positives in the analysis of quinolones residues using liquid chromatography/triple quadrupole mass spectrometry

文献类型： 外文期刊

作者： Lijuan Wang;Hua Yan;Linlin Jiang;Shuilin Cai;Haixin Liu

作者机构：

关键词： False positive;Pefloxacin;Quinolone;Residues;Triple quadrupole tandem mass spectrometry

期刊名称： Microchemical Journal

ISSN： 0026-265X

年卷期： 2025 年 213 卷

页码：

收录情况： SCIE（2025版）

摘要： Quinolone residues in food products pose potential risks to human health, prompting most countries to establish maximum residue limits (MRLs) for these compounds. Currently, triple quadrupole tandem mass spectrometry (QqQ MS) is widely used by testing institutions to screen quinolone residues according to regulatory standards. However, during our current study on pefloxacin detection in sea cucumber, a false positive result was identified using QqQ MS. Then we employed a high-performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) to investigate the interferents in sea cucumber samples. The results from both primary mass spectra (providing accurate mass information) and secondary mass spectra (offering detailed fragmentation data) confirmed the identification of a ciprofloxacin isotope as the interferent. To address this interference issue and enhance the accuracy of pefloxacin detection using low-resolution QqQ MS, three improvement strategies were explored in present work. The first strategy was to optimize the LC separation conditions for enhancing the degree of separation to minimize interference, while the second approach was to introduce a third transition product ion and evaluate the corresponding second ion ratio for better specificity. The third one was to choose the proper product ions with significantly different ionic strengths at the same collision energy for better selectivity. Since low-resolution QqQ MS is commonly utilized by testing organizations for preliminary screening of drug residues, these methodologies present a valuable advancement in enhancing detection accuracy of quinolones in complex matrices. This study not only improves current detection methods but also offers a reference approach for eliminating false positives in the analysis of other pharmaceuticals.

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