Study on the impurity profiles of cloxacillin and flucloxacillin based on liquid chromatography tandem ion trap/time-of-flight mass spectrometry

IF 1.8 3区化学 Q4 BIOCHEMICAL RESEARCH METHODS Rapid Communications in Mass Spectrometry Pub Date : 2024-06-18 DOI:10.1002/rcm.9840

Bingyong Xu, Jiarui Gao, Jian Wang, Fan Wang

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Abstract

Rationale

Cloxacillin and flucloxacillin are prone to degradation and polymerization in humid and hot environments, and their polymers have long been recognized to trigger allergic manifestations. A series of the degradation and polymerized impurities in cloxacillin and flucloxacillin were separated and characterized to ensure safe use of these drugs by the public.

Methods

By studying the chromatographic behavior of the degradation impurities and polymerized impurities in reversed-phase high-performance liquid chromatography (RP-HPLC) gradient elution, the impurities in cloxacillin and flucloxacillin were effectively separated and eluted. RP-HPLC tandem ion trap/time-of-flight mass spectrometry (MS) was applied to characterize the structures of unknown impurities eluted from the RP-HPLC methods for cloxacillin and flucloxacillin. The mechanisms of formation of the impurities in cloxacillin and flucloxacillin were also investigated.

Results

The structures of 10 unknown impurities in cloxacillin and 8 unknown impurities in flucloxacillin were elucidated based on the high-resolution MSⁿ data at positive and negative modes, respectively. Six polymerized impurities were found and characterized, of which three were from the polymerization of cloxacillin and three were from the polymerization of flucloxacillin.

Conclusions

The study on the impurity profiles of cloxacillin and flucloxacillin provided a scientific basis for improving their production processes and quality control.

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基于液相色谱串联离子阱/飞行时间质谱法的氯唑西林和氟氯西林杂质谱研究

理由：氯唑西林和氟氯唑西林在潮湿和炎热的环境中容易降解和聚合，其聚合物长期以来一直被认为会引发过敏表现。为了确保公众安全使用这些药物，我们对氯唑西林和氟氯西林中的一系列降解和聚合杂质进行了分离和鉴定：通过研究降解杂质和聚合杂质在反相高效液相色谱（RP-HPLC）梯度洗脱中的色谱行为，有效地分离和洗脱了氯唑西林和氟氯西林中的杂质。应用 RP-HPLC 串联离子阱/飞行时间质谱（MS）分析了氯唑西林和氟氯西林 RP-HPLC 方法洗脱出的未知杂质的结构。同时还研究了这些杂质在氯唑西林和氟氯西林中的形成机制：结果：根据正、负模式的高分辨率 MSn 数据，分别阐明了氯唑西林中 10 个未知杂质和氟氯西林中 8 个未知杂质的结构。发现并鉴定了 6 个聚合杂质，其中 3 个来自氯唑西林的聚合，3 个来自氟氯西林的聚合：对氯唑西林和氟氯西林杂质谱的研究为改进其生产工艺和质量控制提供了科学依据。

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来源期刊

Rapid Communications in Mass Spectrometry 化学-分析化学

CiteScore

4.10

自引率

5.00%

发文量

219

审稿时长

2.6 months

期刊介绍： Rapid Communications in Mass Spectrometry is a journal whose aim is the rapid publication of original research results and ideas on all aspects of the science of gas-phase ions; it covers all the associated scientific disciplines. There is no formal limit on paper length ("rapid" is not synonymous with "brief"), but papers should be of a length that is commensurate with the importance and complexity of the results being reported. Contributions may be theoretical or practical in nature; they may deal with methods, techniques and applications, or with the interpretation of results; they may cover any area in science that depends directly on measurements made upon gaseous ions or that is associated with such measurements.