Analysis of polymerized impurities in mezlocillin sodium and sulbenicillin sodium using two chromatographic separation mechanisms coupled to tandem mass spectrometry

Ren, Xiaojuan; Tang, Kaixian; Zhou, Ping; Wang, Jian

doi:10.1016/j.jpba.2022.114584

Cited by 13 publications

(6 citation statements)

References 8 publications

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“…A amostra final foi composta por 12 artigos, todos estavam no idioma inglês. Quanto ao país de origem das pesquisas, observou-se predominância na amostra de estudos na China, com seis artigos (JIN et al, 2018;FANG et al, 2020;CHAN et al, 2021;REN et al, 2022;WANG, T. et al, 2022;WANG, Z. et al, 2022). Outros países presentes na amostra foram: Estados Unidos (GOLLAPALLI et al, 2019;ACHANTA et al, 2022) Alguns estudos citam, fora a fabricação inadequada, a indevida consideração aos medicamentos genéricos, como diazepam, risperidona e clozapina.…”

Section: Materials E Métodounclassified

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Impactos Funcionais E Cardiorrespiratórios Pós-Covid-19

Nunes¹,

Santos²,

Macedo³

et al. 2022

Saúde: Impasses E Desafios Enfrentados No Brasil 2

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Editora Direitos para esta edição cedidos à Atena Editora pelos autores. Open access publication by Atena Editora Todo o conteúdo deste livro está licenciado sob uma Licença de Atribuição Creative Commons. Atribuição-Não-Comercial-NãoDerivativos 4.0 Internacional (CC BY-NC-ND 4.0). O conteúdo dos artigos e seus dados em sua forma, correção e confiabilidade são de responsabilidade exclusiva dos autores, inclusive não representam necessariamente a posição oficial da Atena Editora. Permitido o download da obra e o compartilhamento desde que sejam atribuídos créditos aos autores, mas sem a possibilidade de alterála de nenhuma forma ou utilizá-la para fins comerciais.Todos os manuscritos foram previamente submetidos à avaliação cega pelos pares, membros do Conselho Editorial desta Editora, tendo sido aprovados para a publicação com base em critérios de neutralidade e imparcialidade acadêmica.A Atena Editora é comprometida em garantir a integridade editorial em todas as etapas do processo de publicação, evitando plágio, dados ou resultados fraudulentos e impedindo que interesses financeiros comprometam os padrões éticos da publicação. Situações suspeitas de má conduta científica serão investigadas sob o mais alto padrão de rigor acadêmico e ético.

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Section: Materials E Métodounclassified

“…Onde os farmacêuticos tornam-se peças-chaves e devem ainda serem capazes de realizar o controle de qualidade via testes rápidos de eficácia antimicrobiana. Visando determinar, inclusive, o nível de crescimento microbiano que uma droga é capaz de suportar (REN et al, 2022).…”

Section: Materials E Métodounclassified

Impactos Funcionais E Cardiorrespiratórios Pós-Covid-19

Nunes¹,

Santos²,

Macedo³

et al. 2022

Saúde: Impasses E Desafios Enfrentados No Brasil 2

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“…However, it can only control the total amount of polymerized impurities, with low column efficiency, poor resolution, and long separation time. Compared with GFC, the high‐performance size exclusion chromatography (HPSEC) method and the reversed‐phase, high‐performance liquid chromatography (RP‐HPLC) method have the advantages of high separation efficiency, high sensitivity, and short analysis time 9–12 …”

Section: Introductionmentioning

confidence: 99%

“…Compared with GFC, the highperformance size exclusion chromatography (HPSEC) method and the reversed-phase, high-performance liquid chromatography (RP-HPLC) method have the advantages of high separation efficiency, high sensitivity, and short analysis time. [9][10][11][12] The RP-HPLC method was used to determine related substances in drugs, and GFC/HPSEC method was used for quantitative analysis of the polymerized impurities in cefamandole nafate in the reported literature, [13][14][15][16][17][18] but the impurity profile and the structures of polymerized impurities were not studied systematically and characterized using HPLC-MS. 19 In this study, reverse phase high-performance liquid (Shanghai, China). Water was deionized and further purified using a Millipore Milli-Q-Gradient purification system (Millipore, Waters, Milford, MA, USA).…”

Section: Introductionmentioning

confidence: 99%

Impurity profile and spectrum characteristics of the isomers in cefamandole nafate using high‐ performance liquid chromatography/high‐performance size exclusion chromatography tandem ion trap/time‐of‐flight mass spectrometry

Wang

Gao

Chen

et al. 2022

Rapid Comm Mass Spectrometry

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Rationale Reversed‐phase, high‐performance liquid chromatography (RP‐HPLC) and high‐performance size exclusion chromatography (HPSEC) methods were developed to effectively separate unknown impurities and polymerized impurities in cefamandole nafate. The liquid chromatography‐tandem ion trap/time‐of‐flight mass spectrometry (LC‐IT‐TOF‐MS) was applied to characterize the structures of the impurities. Ultraviolet (UV) spectrum characteristics and mass spectrum characteristics of △3‐isomer and 7‐epimer in cefamandole nafate were studied to distinguish the isomers. Methods RPLC‐IT‐TOF‐MS was used to characterize the structures of unknown impurities and polymerized impurities eluted from the C18 column. On this basis, the two‐dimensional (2D) HPSEC‐IT‐TOF‐MS was used to confirm the structures of polymerized impurities eluted from the TSK‐gel G2000SWxl column. Complete fragmentation patterns of impurities were studied and used to obtain information about the structures of the impurities. Results The structures of 19 unknown impurities in cefamandole nafate were elucidated based on the high‐resolution MSn data with both positive and negative modes, assisted by the UV spectra and stress testing, of which 2 impurities were polymerized impurities. Cefamandole nafate produced a series of degradation impurities, and another principal component cefamandole acid also produced a series of similar degradation impurities. The disciplines between mass fragmentation pattern/UV spectrum and structure for △3‐isomer and 7‐epimer were presented to distinguish their structures. Conclusions The results of this study provided a scientific basis for the improvement of official monographs in pharmacopoeias to effectively control the impurities and ensure drug safety for the public. This study also revealed the formation mechanisms of degradation impurities in cefamandole nafate, which may guide industry to improve the manufacturing process and storage conditions to reduce the content of impurities in products.

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“…Furthermore, RP-HPLC-MS can also be used to analyze polymerized impurities. [20][21][22] For cloxacillin and flucloxacillin, various analytical techniques have been developed to estimate the quality of pharmaceuticals. [23][24][25][26] However, the impurity profile and the structures of many polymerized impurities in cloxacillin and flucloxacillin were not studied systematically and characterized using RP-HPLC-MS.…”

mentioning

confidence: 99%

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

Xu,

Gao,

Wang

et al. 2024

Rapid Comm Mass Spectrometry

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RationaleCloxacillin 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.MethodsBy 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.ResultsThe 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.ConclusionsThe 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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Analysis of polymerized impurities in mezlocillin sodium and sulbenicillin sodium using two chromatographic separation mechanisms coupled to tandem mass spectrometry

Cited by 13 publications

References 8 publications

Impactos Funcionais E Cardiorrespiratórios Pós-Covid-19

Impactos Funcionais E Cardiorrespiratórios Pós-Covid-19

Impurity profile and spectrum characteristics of the isomers in cefamandole nafate using high‐ performance liquid chromatography/high‐performance size exclusion chromatography tandem ion trap/time‐of‐flight mass spectrometry

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

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