A LC-MS/MS method for simultaneous estimation of a novel anti-diabetic combination of saxagliptin and dapagliflozin using a polarity switch approach: application to in vivo rat pharmacokinetic study

2019 ◽  
Vol 11 (2) ◽  
pp. 219-226 ◽  
Author(s):  
Shruti Surendran ◽  
David Paul ◽  
Sunil Pokharkar ◽  
Abhijeet Deshpande ◽  
Sanjeev Giri ◽  
...  

First LC-MS/MS method for the simultaneous determination of SAX and DAP. The method offers good sensitivity with LLOQ of 0.2 ng mL−1 for SAX and 5 ng mL−1 for DAP.

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1662
Author(s):  
Wenlong Wei ◽  
Yang Yu ◽  
Xia Wang ◽  
Linhui Yang ◽  
Hang Zhang ◽  
...  

Characterization and determination of metabolites to monitor metabolic pathways play a paramount role in evaluating the efficacy and safety of medicines. However, the separation and quantification of metabolites are rather difficult due to their limited contents in vivo, especially in the case of Chinese medicine, due to its complexity. In this study, an effective and convenient method was developed to simultaneously quantify bufalin and its nine metabolites (semi-quantitation) in rat plasma after an oral administration of 10 mg/kg to rats. The prototype and metabolites that were identified were subsequently quantified using positive electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m/z 387.4→369.6 and 387.4→351.3 for bufalin, m/z 513.7→145.3 for IS, and 387.4→369.6, 419.2→365.2, and 403.2→349.2 for the main metabolites (3-epi-bufalin, dihydroxylated bufalin, and hydroxylated bufalin, respectively). The method was validated over the calibration curve range of 1.00–100 ng/mL with a limit of quantitation (LOQ) of 1 ng/mL for bufalin. No obvious matrix effect was observed, and the intra- and inter-day precisions, as well as accuracy, were all within the acceptable criteria in this method. Then, this method was successfully applied in metabolic profiling and a pharmacokinetic study of bufalin after an oral administration of 10 mg/kg to rats. The method of simultaneous determination of bufalin and its nine metabolites in rat plasma could be useful for pharmacokinetic–pharmacodynamic relationship research of bufalin, providing experimental evidence for explaining the occurrence of some adverse effects of Venenum Bufonis and its related preparations.


RSC Advances ◽  
2015 ◽  
Vol 5 (95) ◽  
pp. 78336-78351 ◽  
Author(s):  
Wei Liu ◽  
Dandan He ◽  
Yudan Zhu ◽  
Xuemei Cheng ◽  
Hao Xu ◽  
...  

An UPLC-MS/MS method was developed to simultaneously determinate vasicine and its main metabolites and applied to the pharmacokinetic study. In addition, the anti-butyrylcholinesterase activity of component in plasma was evaluatedin vitro.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


1975 ◽  
Vol 21 (3) ◽  
pp. 428-431 ◽  
Author(s):  
Godfrey Moses ◽  
Edwin Olivero ◽  
Thomas F Draisey

Abstract An isopropanolic extract of serum can be made suitable for the simultaneous estimation of cholesterol and triglycerides by passing it through a commercially-available chromatographic column containing activated metallic oxides in which alumina predominates. No centrifugation step nor phase separation is required. Use of the purified extract allows existing methods to be simplified and shortened without loss of reproducibility or stability. Results compare well with those obtained by traditional methods.


Bioanalysis ◽  
2014 ◽  
Vol 6 (18) ◽  
pp. 2343-2356 ◽  
Author(s):  
Jiangbo Du ◽  
Zhiyu Ma ◽  
Yifan Zhang ◽  
Ting Wang ◽  
Xiaoyan Chen ◽  
...  

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