An integrated approach for detection and characterization of the trace impurities in levofloxacin using liquid chromatography-tandem mass spectrometry

Zheng, Yan; Zhang, Ruiping; Wang, Yucheng; Wang, Juxian; Wang, Huiqing; Wu, Yang-feng; He, Wen‐Yi; Abliz, Zeper

doi:10.1002/rcm.6886

Cited by 13 publications

(4 citation statements)

References 29 publications

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“…Different impurities lead to different toxicity, so it is necessary to investigate the photodegradation impurity profile in lomefloxacin hydrochloride ear drops. Various techniques like high‐performance liquid chromatography (HPLC) coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, liquid chromatography coupled with nuclear magnetic resonance, etc., have been used in the pharmaceutical industries for the identification and characterization of impurities in drugs 16–18 . Among them, ion trap/time‐of‐flight mass spectrometry (IT‐TOFMS) not only can allow accurate molecular weights to be obtained, but also allows multistage mass spectrometry analysis, which can lead to more information on the molecular structure of impurities.…”

Section: Introductionmentioning

confidence: 99%

Study of the impurity profile of photodegradation in lomefloxacin hydrochloride ear drops using liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry

Zeng,

Yang,

Gao

et al. 2024

Rapid Comm Mass Spectrometry

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RationaleLomefloxacin hydrochloride ear drops are highly unstable to light and prone to produce photodegradation impurities. These impurities might be related to the phototoxicity of lomefloxacin, which could seriously threaten the health of patients. In this article, the photodegradation impurity profile in lomefloxacin hydrochloride ear drops was studied for further improvement of quality control of the drug.MethodsBy studying the chromatographic behavior of photodegradation impurities, the photodegradation impurities in lomefloxacin hydrochloride ear drops were separated and detected effectively. Liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry was applied to characterize the structures of the photodegradation impurities in lomefloxacin hydrochloride ear drops.ResultsThe structures of 17 impurities in lomefloxacin hydrochloride ear drops were elucidated based on high‐resolution MSn data in positive ion mode, 12 of them being unknown impurities.ConclusionsThe structural characteristics and fragmentation patterns of the photodegradation impurities were also studied. The study of the photodegradation impurity profile in lomefloxacin hydrochloride ear drops provides a scientific basis for quality control of these ear drops and ensures the safety of drug use by the public.

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Section: Introductionmentioning

confidence: 99%

Study of the impurity profile of photodegradation in lomefloxacin hydrochloride ear drops using liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry

Zeng,

Yang,

Gao

et al. 2024

Rapid Comm Mass Spectrometry

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“…Hence, it is necessary to assess the stability of the drug under various forced degradation conditions and develop an efficient analytical method for the analysis of all DPs. Hyphenated techniques such as liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI‐MS/MS) combined with accurate mass measurement have been established as promising techniques and widely used in the identification and structural elucidation of DPs …”

mentioning

confidence: 99%

“…Hyphenated techniques such as liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) combined with accurate mass measurement have been established as promising techniques and widely used in the identification and structural elucidation of DPs. [13][14][15] A thorough literature survey revealed the availability of only a few analytical methods like HPLC [16] and LC/MS/MS for the determination of SQM in biological samples. [17][18][19] However, no analytical method has been reported for the determination of SQM and its DPs in bulk and pharmaceutical formulations.…”

mentioning

confidence: 99%

Identification of degradation products of saquinavir mesylate by ultra‐high‐performance liquid chromatography/electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry and its application to quality control

Thummar

Patel

Petkar

et al. 2017

Rapid Comm Mass Spectrometry

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Rationale Saquinavir mesylate (SQM) is an antiviral drug used for the treatment of HIV infections. The identification and characterization of all degradation products are essential for achieving the quality in pharmaceutical product development and also for patient safety. Methods The drug was subjected to hydrolytic (HCl, NaOH and water), oxidative (H2O2), photolytic (UV and fluorescence light) and thermal (dry heat) forced degradation conditions as per ICH guidelines. The best chromatographic separation of the drug and all degradation products (DPs) was achieved on a CSH‐Phenyl Hexyl column (100 × 2.1 mm, 1.7 μm) with ammonium acetate (10 mM, pH 5.0) and methanol as mobile phase in gradient mode at a flow rate of 0.28 mL/min. Results Nine DPs were obtained under various forced degradation conditions. All the DPs were characterized by using ultra‐high‐performance liquid chromatography/electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry (UHPLC/ESI‐QTOF MS/MS) and the degradation pathway of the drug was justified by mechanistic explanations. The main DPs were formed by amide hydrolysis, conversion into diastereomers, an N‐oxide and dehydration as well as oxidation of the alcohol from the drug. The method was validated and can be used in a quality control (QC) laboratory to assure the quality of SQM in bulk and finished formulations. Conclusions A simple UHPLC/photodiode array (PDA) method was developed and successfully transferred to UHPLC/ESI‐Q‐TOF MS/MS for the identification and characterization of DPs. Very interestingly, diastereomeric DPs were obtained and successfully resolved by the chromatographic method. Copyright © 2017 John Wiley & Sons, Ltd.

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“…Because LC-MS is one of the leading techniques used in drug metabolism research, due to its high sensitivity and capacity for structure elucidation, − several scan functions, such as IDA, − selected reaction monitoring (SRM), and precursor and neutral loss scan based on triple quadrupole instruments, have their own characteristics and are extensively used in drug metabolism studies. However, these scan functions are relatively insensitive, have a long duty cycle, and require multiple injections to monitor multiple precursors and neutral losses in order to be comprehensive .…”

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confidence: 99%

Targeted Data-Independent Acquisition and Mining Strategy for Trace Drug Metabolite Identification Using Liquid Chromatography Coupled with Tandem Mass Spectrometry

et al. 2015

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Detection and identification of unknown or low-level drug-related metabolites in complex biological materials is an ongoing challenge. A highly selective and sensitive method could be a possible solution. Here, we proposed a targeted data-independent acquisition and mining (TDIAM) strategy for the rapid identification of trace drug metabolites using ultra-high-performance liquid chromatography coupled with high-resolution tandem mass spectrometry (UHPLC-HRMS/MS). In this strategy, raw data is acquired by a novel tm-MS scan, which contains an interleaved full MS scan with a targeted mass range and a product ion scan by selecting all ions in the targeted mass range as precursor ions. For efficient discovery of metabolites, raw data are analyzed by a new postacquisition processing method, Molecule- and Fragmentation-driven Mass Defect Filters (MF-MDFs), which was developed based on the fragmentation of parent drug to pick out molecular ions and fragment ions of potential metabolites from the complex matrix. When applying the proposed strategy to paclitaxel metabolism research, we successfully identified 10 metabolites, among which six were not previously reported. The results demonstrated that TDIAM greatly improved throughput, detective sensitivity, and selectivity and, more importantly, yielded almost the same spectrum as traditional HRMS/MS. Therefore, TDIAM provides structure-enriched evidence to confirm the existence and elucidate the structures of metabolites. This strategy is suitable for identification of metabolites present at low concentrations in a complex matrix, and it has the potential to provide an efficient, sensitive, and labor-saving solution for drug metabolite research.

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An integrated approach for detection and characterization of the trace impurities in levofloxacin using liquid chromatography-tandem mass spectrometry

Cited by 13 publications

References 29 publications

Study of the impurity profile of photodegradation in lomefloxacin hydrochloride ear drops using liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry

Study of the impurity profile of photodegradation in lomefloxacin hydrochloride ear drops using liquid chromatography combined with ion trap/time‐of‐flight mass spectrometry

Identification of degradation products of saquinavir mesylate by ultra‐high‐performance liquid chromatography/electrospray ionization quadrupole time‐of‐flight tandem mass spectrometry and its application to quality control

Targeted Data-Independent Acquisition and Mining Strategy for Trace Drug Metabolite Identification Using Liquid Chromatography Coupled with Tandem Mass Spectrometry

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