Green Simultaneous Chromatographic Separation of Pyridostigmine Bromide and Its Related Substances in Pure Form, Tablets and Spiked Human Plasma

2019 ◽  
Vol 57 (7) ◽  
pp. 653-661
Author(s):  
Ibrahim A Naguib ◽  
Eglal A Abdelaleem ◽  
Aml A Emam ◽  
Fatma F Abdallah
Keyword(s):  
Acetic Acid ◽  
Quantitative Determination ◽  
Human Plasma ◽  
High Performance ◽  
Pyridostigmine Bromide ◽  
Pharmacokinetic Studies ◽  
Related Substances ◽  
Ich Guidelines ◽  
Developing System

Abstract A green, accurate and specific high-performance thin-layer chromatographic (HPTLC) method was developed and validated for simultaneous quantitative determination of pyridostigmine bromide (PR), impurity B (IMP B);3-hydroxy-N-methylpyridinium bromide and impurity A (IMP A); pyridin-3-yl-dimethylcarbamate. The two pharmacopeial impurities are also its main inactive metabolites. Furthermore, IMP B is known to be its alkaline-induced degradation product. Achievable separation of the studied components required silica gel HPTLC F254 plates as a stationary phase and acetone: acetic acid (80:20, v/v) as a developing system. Scanning of the separated bands was done at 260 nm. According to green solvent selection guidelines, acetone and acetic acid are eco-friendly solvents. Validation of the developed method was insured by its acquiesce to international conference on harmonization (ICH) guidelines. The introduced method was successfully achieved for the quantitative determination of PR, IMP B and IMP A in the range of 0.4–10, 2–11 and 0.4–3.5 μg/band, respectively. Successful application of the developed method was done for determination of PR in human plasma in the range of 0.6–10 μg/band, so the proposed HPTLC can be applied in the pharmacokinetic studies. The studied drug was also analyzed in Mestinon® tablets using the developed method.

HPTLC Separation of a Hepatoprotective Combination in Pharmaceutical Formulation and Human Plasma

2020 ◽  
Vol 58 (5) ◽  
pp. 411-417
Author(s):  
Maimana A Magdy ◽  
Rehab M Abdelfatah
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Spiked Plasma ◽  
Significant Difference ◽  
Developing System

Abstract A binary mixture of Silymarin (SR) and Vitamin E (VE) acetate, of an antioxidant and a hepatoprotective effect, has been analyzed using a sensitive, selective and economic high performance thin layer chromatographic (HPTLC) method in their pure forms, pharmaceutical formulation and spiked human plasma. SR and VE were separated on 60F254 silica gel plates using hexane:acetone:formic acid (7:3:0.15, v/v/v) as a developing system with UV detection at 215 nm. The method was evaluated for linearity, accuracy, precision, selectivity, limit of detection (LOD) and limit of quantification (LOQ). SR and VE were detected in the linear range of 0.2–2.5 and 0.2–4.5 μg/band, respectively. Method validation was done as per ICH guidelines and acceptable results of accuracy of 99.86 ± 1.190 and 100.22 ± 1.609 for SR and VE, respectively were obtained. The method has been successfully applied for determination of the studied drugs in their pharmaceutical formulation without any interference from excipients, and in spiked plasma samples. Results obtained by the developed HPTLC-densitometric method were statistically compared to those obtained by the reported HPLC methods and no significant difference was found between them.

AN EFFICIENT HPLC-UV METHOD FOR THE QUANTITATIVE DETERMINATION OF CEFADROXIL IN HUMAN PLASMA AND ITS APPLICATION IN PHARMACOKINETIC STUDIES

2012 ◽  
Vol 35 (13) ◽  
pp. 1871-1881 ◽  
Author(s):  
Eunice Kazue Kano ◽  
Cristina Helena dos Reis Serra ◽  
Eunice Emiko Mori Koono ◽  
Kazuo Fukuda ◽  
Valentina Porta
Keyword(s):  
Quantitative Determination ◽  
Human Plasma ◽  
Pharmacokinetic Studies

scholarly journals Validated LC–MS/MS Assay for the Quantitative Determination of Fimasartan in Human Plasma: Application to Pharmacokinetic Studies

2015 ◽  
Vol 53 (8) ◽  
pp. 1250-1256 ◽  
Author(s):  
Seo Hyun Yoon ◽  
Seul Oh ◽  
Hwa Suk Kim ◽  
SoJeong Yi ◽  
Kyung-Sang Yu ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
Human Plasma ◽  
Pharmacokinetic Studies

LC–MS–MS Quantitative Determination of Ursolic Acid in Human Plasma and Its Application to Pharmacokinetic Studies

2010 ◽  
Vol 72 (11-12) ◽  
pp. 1107-1113 ◽  
Author(s):  
Zhi-Rong Tan ◽  
Yao Chen ◽  
Gan Zhou ◽  
Shan Cao ◽  
Xiang-Dong Peng ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
Human Plasma ◽  
Ursolic Acid ◽  
Pharmacokinetic Studies

scholarly journals A reliable HPLC-DAD method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient

2020 ◽  
Vol 32 (2) ◽  
pp. 80-85
Author(s):  
Tingting Zhang ◽  
Wanting Yin ◽  
Bo Jin ◽  
Tong Li ◽  
Chen Ma
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Active Pharmaceutical Ingredient ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Phase System ◽  
Related Substances ◽  
Ich Guidelines ◽  
Bulk Drug

A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

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