Structural characterization of low level degradants in aztreonam injection and an innovative approach to aid HPLC method validation

2016 ◽  
Vol 124 ◽  
pp. 358-364 ◽  
Author(s):  
Qingmei Ye ◽  
Wei Ding ◽  
Frank Rinaldi ◽  
Yande Huang ◽  
Scott A. Miller ◽  
...  
2013 ◽  
Vol 110 ◽  
pp. 665-674 ◽  
Author(s):  
Mariana Mirelle Pereira Natividade ◽  
Luiz Claudio Corrêa ◽  
Scheilla Vitorino Carvalho de Souza ◽  
Giuliano Elias Pereira ◽  
Luiz Carlos de Oliveira Lima

2012 ◽  
Vol 7 (9) ◽  
pp. 1934578X1200700 ◽  
Author(s):  
Somendu K. Roy ◽  
Amit Srivastava ◽  
Sanjay M. Jachak

The roots of Caesalpinia digyna have been reported to contain gallic acid derivatives and minor homoisoflavonoids, but HPLC-ESI-MS and HPLC analyses of the homoisoflavonoids were challenging due to their low concentration in the roots. Separation and identification was accomplished by HPLC-ESI-MS and further elaborated for quantification using a C18 column with detection at 330 nm. A gradient mobile phase consisting of methanol and water (0.1% acetic acid) was used. The developed HPLC method showed good linearity (r2≥0.998), high precision (RSD<5%) and a good recovery (99.3-104.5%) of the compounds. The lowest detection limit was 0.75 ng and the method was found to be robust. All the validation parameters were found to be within the permissible limits and, therefore, the developed method is accurate and reliable for the quality control of C. digyna and other Caesalpinia species. This is the first report of sample preparation on Diaion HP-20 resin and characterization of homoisoflavonoids by HPLC-ESI-MS, extended by extensive quantitative HPLC analysis of homoisoflavonoids in C. digyna roots and method validation.


2018 ◽  
Vol 66 ◽  
pp. 160-167 ◽  
Author(s):  
Emanuela Monteiro Coelho ◽  
Carla Valéria da Silva Padilha ◽  
Gabriela Aquino Miskinis ◽  
Antônio Gomes Barroso de Sá ◽  
Giuliano Elias Pereira ◽  
...  

2019 ◽  
Vol 56 (10) ◽  
pp. 4575-4584 ◽  
Author(s):  
Marcos dos Santos Lima ◽  
Polyana Campos Nunes ◽  
Bernadete de Lourdes de Araújo Silva ◽  
Carla Valéria da Silva Padilha ◽  
Thaís Helena Figueiredo do Bonfim ◽  
...  

2017 ◽  
Vol 133 ◽  
pp. 15-26 ◽  
Author(s):  
Ajay Kumar ◽  
Subba Rao Devineni ◽  
Shailender Kumar Dubey ◽  
Pradeep Kumar ◽  
Vishal Srivastava ◽  
...  

Author(s):  
S. F. Hayes ◽  
M. D. Corwin ◽  
T. G. Schwan ◽  
D. W. Dorward ◽  
W. Burgdorfer

Characterization of Borrelia burgdorferi strains by means of negative staining EM has become an integral part of many studies related to the biology of the Lyme disease organism. However, relying solely upon negative staining to compare new isolates with prototype B31 or other borreliae is often unsatisfactory. To obtain more satisfactory results, we have relied upon a correlative approach encompassing a variety EM techniques, i.e., scanning for topographical features and cryotomy, negative staining and thin sectioning to provide a more complete structural characterization of B. burgdorferi.For characterization, isolates of B. burgdorferi were cultured in BSK II media from which they were removed by low speed centrifugation. The sedimented borrelia were carefully resuspended in stabilizing buffer so as to preserve their features for scanning and negative staining. Alternatively, others were prepared for conventional thin sectioning and for cryotomy using modified procedures. For thin sectioning, the fixative described by Ito, et al.


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