scholarly journals Practical Implication of Chromatographic Method for Estimation of Aceclofenac and Pregabalin in Bulk and Pharmaceutical Dosage Forms

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Hitendrakumar D. Gelani ◽  
Payal P. Chauhan ◽  
Samir K. Shah

Background. Aceclofenac and Pregabalin in combination significantly reduce pain as compared to individual drug in chronic low back pain. Literature reveals that all the reported spectrophotometric methods either need tedious extraction procedures, do not offer high sensitivity, use nonspecific reagent, or recommend the measurement of absorbance in the near UV region where interference most probably occurs that does not offer suitable linearity range. Result. A selective, sensitive, accurate, and precise, high performance liquid chromatographic method with UV detector analysis of Aceclofenac and Pregabalin was investigated. Good chromatographic separation was achieved using an ODS-BP hypersil C18 column (250 mm × 4.6 mm, i.d., 5 μm) and a mobile phase consisting of 0.05 M phosphate buffer (KH2PO4) (pH 6.0) : methanol (60 : 40, v/v) at a flow rate 1 mL/min. The ultraviolet detector was set at wavelength 218 nm. Retention time for Aceclofenac and Pregabalin was found to be 3.220 and 5.910 min, respectively. Rectilinear relationship with good regression coefficients 0.999 and 0.999 was found over the concentration ranges of 5–25 μg/mL and 3.75–18.75 μg/mL for ACF and PGB, respectively, with detection limits 0.64 and 0.35 μg/mL and quantitation limits 1.95 and 1.06 μg/mL. Conclusion. The mean percentage recoveries were in the range of 98.45–100.08 and 99.69–100.48 for ACF and PGB, respectively. The developed method was successfully applied to the analysis of the drugs in their commercial tablets.

Author(s):  
D C Sampson ◽  
R M Fox ◽  
M H N Tattersall ◽  
W J Hensley

A fast, simple, precise, high-performance liquid chromatographic method for the assay of 5-fluorouracil in plasma from humans receiving continuous intravenous infusion is described. After a single extraction, underivatised 5-fluorouracil is assayed by high-performance liquid chromatography using a variable-wavelength ultraviolet detector. After extraction of 1 ml plasma, 0·3 μmol/l can be assayed. The assay is reproducible and linear up to at least 40 μmol/l. A single determination takes 3 hours and a batch of 40 specimens can be extracted and assayed in 4 working hours if automated equipment is used, enabling injections and calculations to be done overnight.


Author(s):  
Shivani Kalokhe ◽  
Santaji Nalwade ◽  
Pallavi Patil ◽  
Poonam Raskar

Abstract A novel, delicate, stability-indicating, gradient, reversed-phase high-performance liquid chromatographic method has been established for the quantitative estimation of methocarbamol (MTC) and its impurities present in a pharmaceutical oral suspension. XBridge C18, 5 μm, 250 mm × 4.6 mm column was used to accomplish chromatographic separation with a buffered mobile phase consisting of a mixture of 0.01 M of sodium dihydrogen phosphate (pH 7.0 buffer) and methanol in the ratio of 95:05 (v/v), respectively, were used as solvent A and a mixture of methanol and Milli-Q water in the ratio 90:10 (v/v), respectively, was used as solvent B. Analysis was carried out at 0.8 mL/min flow rate and the detection wavelength at 225 nm. The compartment temperature of the column is put at 25°C. The resolution of MTC and its four impurities has been attained >2.0 for all pairs of compounds. Significant degradation of MTC was photolytic, thermal and oxidative stress conditions. Validation of the developed method was performed as stated by the International Conference on Harmonization guidelines with regard to all validation parameters like specificity, accuracy, linearity, precision, limit of detection, limit of quantitation and robustness.


2020 ◽  
Vol 15 (3) ◽  
pp. 127-135

The present study describes the optimization and validation of a high-performance liquid chromatographic (HPLC) method for the determination of seven medicines (Metformin hydrochloride, Vildagliptin, Gliclazide, Sitagliptin phosphate, Pioglitazone hydrochloride, Glibenclamide and Glimepirde) in bulk and pharmaceutical dosage forms. The chromatographic separation could be achieved using a C8 column (100 Å, 5 µm, 150 mm) at 30 °C. Thereby, the mobile phase is a mixture of acetonitrile and an aqueous solution of triethylamine (0.5% v/v) and phosphoric acid 10% w/v (pH 7.0) at a mixing ratio of 32.5:67.5 v/v%, with a flow rate of 1.0 ml/min and detection performed at 210 nm using a UV detector. The results were found satisfactory and the method can be adapted to routine quality control of medications as recommended by the guidelines of the International Conference on Harmonization.


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