scholarly journals Efficient Validated HPLC/UV Method for Determination of Valsartan and Atenolol in Dosage Form And In Vitro Dissolution Studies

2020 ◽  
Vol 10 (6) ◽  
pp. 6669-6675

The main purpose of this study was to develop and validate an efficient HPLC/UV method for determination of valsartan and atenolol and to introduce the dissolution profiles of tablets; The resolution of peaks was best achieved with Zorbax C8 (4.6 mm i.d. X 150 mm, 5 μm) column. Samples were chromatographed in a isocratic mode (methanol and 25 mM solution potassium dihydrogen phosphate pH 7.3 (55:45, V/V)), pumped with 1.0 mL/min at 40 °C set temperature of column oven, with UV detector set to 225 nm wavelength; The total chromatographic run time was 6 minutes. The retention time of valsartan is 1.753 min, atenolol – 3.064 min. Linearity was examined and proven at different concentration levels in the range of working concentration of valsartan ( 0.16-0.96 mg/mL) and atenolol (0.2–1.2 mg/mL). The high value of recoveries obtained for valsartan and atenolol indicates that the proposed method was found to be accurate. In all three dissolution media the releases of valsartan and atenolol are more than 85% in 15 min A rapid, simple, accurate, selective, and sensitive method was developed for the determination of valsartan and atenolol in dosage forms. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine quality control of drugs and in vitro dissolution study.

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (02) ◽  
pp. 44-49
Author(s):  
P Choksi ◽  
◽  
F. Shaikh ◽  
D. A. Shah ◽  
K. Agarwal ◽  
...  

A simple, specific, accurate, precise and reproducible method has been developed and validated for the estimation of bromhexine hydrochloride and enrofloxacin in fixed dose combination using RP-HPLC. The separation was achieved using stationary phase ODS Hypersil C18 column (250 mm× 4.6 mm i.d.) in isocratic mode, with mobile phase containing 0.05 M potassium dihydrogen phosphate buffer (pH 4 by o-phosphoric acid) : methanol: acetonitrile : triethylamine (40:20:40:01), at a flow rate of 1.0mL/min and eluents were monitored at 256 nm. The retention time of enrofloxacin and bromhexine HCl were found to be 3.00 min and 5.1 min respectively. The linearity for bromhexine HCl and enrofloxacin was in the range of 2-15 μg/mL and 20-150 μg/mL, respectively. The method was validated as per ICH guideline. The recoveries of bromhexine HCl and enrofloxacin were found in the range of 99.61-101.65% and 99.52-100.13 %, respectively. The method was successfully applied for the determination of both the drugs in combined dosage form.


INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (11) ◽  
pp. 24-28
Author(s):  
S.B Rohith ◽  
◽  
B.M Gurupadayya ◽  
R.S Chandan

A novel ultra-fast liquid chromatography (RP- UFLC) analytical method has been developed to quantify opipramol in tablet formulations. The determination was carried out by means of a Phenomenex Luna C8 Column (250×4.60mm, 5μ); potassium dihydrogen phosphate buffer of pH 2.4 and acetonitrile was used as a mobile phase in the ratio of 60:40 V/V with a flow rate of 1.00 mL/min. The photo diode array (PDA) detector was operated at wavelength of 253nm. The retention time for opipramol was found to be 2.72min. The validation studies were carried out according to ICH guidelines with a specific aim to establish that the new analytical method developed complied with the validation guidelines. The main parameters for validation study are specificity, linearity, accuracy, precision, LOD, LOQ and robustness. This method can be used for quality control analysis of opipramol in pure and marketed formulation.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Zhikui Yin ◽  
Suying Ma ◽  
Jincai Wang ◽  
Xiaojun Shang

A simple, sensitive, and accurate RP-HPLC coupled with UV detector method was developed and validated for simultaneous determination of matrine and tinidazole in compound lotion. The chromatographic separation of the two compounds was carried out with a SinoChoom ODS-BP C18column (5 μm, 4.6 mm × 200 mm) analytical column, using a mobile phase consisting of 0.025 mol/L potassium dihydrogen phosphate (containing triethylamine 0.05%, v/v) and acetonitrile (80 : 20, v/v) at a flow rate of 1.0 mL/min. The detection was monitored at 210 and 310 nm for matrine and tinidazole, respectively. Total run time was 12 min, and the column was maintained at 25°C. The excipients in the compound lotion did not interfere with the drug peaks. The calibration curves of matrine and tinidazole were fairly linear over the concentration ranges of 10.0–100.0 μg/mL (r=0.9954) and 20.0–200.0 μg/mL (r=0.9968), respectively. The RSD of both the intraday and interday variations was below 1.5% for matrine and tinidazole. The proposed HPLC method was validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of matrine and tinidazole in compound lotion.


2021 ◽  
Vol 11 (5) ◽  
pp. 13089-13101

In this study, a sustainable HPLC-UV-DAD method was developed and validated for the determination of allopurinol in tablets and optimization of the dissolution test using factorial design. The separation of the analyte from the sample matrix was achieved in 3.01 minutes in a C8 column (4.6 mm X 150 mm X 5 μm), using mobile phase 0.1 mol L-1 HCl (25%) + ethanol (50%) + ultrapure water (25%) by UV detection at 249 nm. The method presented satisfactory analytical parameters of validation (specificity, selectivity, linearity, stability, precision, accuracy, and robustness), showing no matrix effects. The dissolution test was optimized by complete factorial design 23 and, the optimal conditions were: HCl 0.001 mol L-1, apparatus II (paddle) and 75 rpm. The analytical procedures and dissolution tests were applied to allopurinol tablets marketed in Bahia, Brazil, to evaluate the dissolution studies. The pharmaceuticals had similar dissolution profiles and first-order dissolution kinetics. This new and sustainable HPLC-UV-DAD method is friendly to the environment and can be used for the routine pharmaceutical analysis of allopurinol in fixed dosage forms.


2015 ◽  
Vol 98 (6) ◽  
pp. 1496-1502 ◽  
Author(s):  
Ramzia I El-Bagary ◽  
Ehab F Elkady ◽  
Shereen Mowaka ◽  
Maria Attallah

Abstract Two simple, accurate, and precise chromatographic methods have been developed and validated for the determination of dronedarone (DRO) HCl and amiodarone (AMI) HCl either alone or in binary mixtures due to the possibility of using AMI as a counterfeit of DRO because of its lower price. First, an RP-HPLC method is described for the simultaneous determination of DRO and AMI. Chromatographic separation was achieved on a BDS Hypersil C18 column (150 × 4.6 mm, 5 μm). Isocratic elution based on potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (10 + 90, v/v) at a flow rate of 2 mL/min with UV detection at 254 nm was performed. The second method is RP ultra-HPLC in which the chromatographic separation was achieved on an AcclaimTM RSLC 120 C18 column (100 × 2.1 mm, 2.2 μm) using isocratic elution with potassium dihydrogen phosphate buffer with 0.1% triethylamine pH 6–methanol (5 + 95, v/v) at a flow rate of 1 mL/min with UV detection at 254 nm. Linearity, accuracy, and precision of the two methods were found to be acceptable over the concentration ranges of 5–80 μg/mL for both DRO and AMI. The results were statistically compared using one-way analysis of variance. The optimized methods were validated and proved to be specific, robust, precise, and accurate for the QC of the drugs in their pharmaceutical preparations.


1967 ◽  
Vol 13 (7) ◽  
pp. 749-753 ◽  
Author(s):  
P. K. Chhonkar ◽  
N. S. Subba-Rao

Phosphate solubilizing ability of different isolates of fungi associated with legume root nodules was studied in vitro. Among the fungi tested, isolates of Penicillium lilacinum, Aspergillus sp., A. flavus, A. niger, A. terreus, and A. nidulans solubilized insoluble tricalcium phosphate. When soluble potassium dihydrogen phosphate was present with tricalcium phosphate in the medium, some of the fungi failed to solubilize phosphate.


2010 ◽  
Vol 48 (9) ◽  
pp. 755-759 ◽  
Author(s):  
C. S. Paim ◽  
M. T. Martins ◽  
M. D. Malesuik ◽  
M. Steppe

2017 ◽  
Vol 100 (6) ◽  
pp. 1869-1878 ◽  
Author(s):  
Bixia Yang ◽  
Lian Wang ◽  
Chunying Luo ◽  
Xixi Wang ◽  
Chengjun Sun

Abstract An analytical method was developed for the simultaneous determination of 11 aminoglycoside (AG) antibiotics, including amikacin, paromomycin, dihydrostreptomycin, gentamicin C1a, hygromycin, kanamycin, netilmicin, spectinomycin, sisomicin, streptomycin, and tobramycin in honey, milk, and pork samples by LC with tandem MS and molecularly imprinted polymer (MIP) SPE. The AG antibiotics in milk and homogenated meat samples were extracted with a solution composed of 10 mmol/L potassium dihydrogen phosphate, 0.4 mmol/L EDTA-Na2, and 2% trichloroacetic acid. For honey samples, the extractant was 50 mmol/L potassium dihydrogen phosphate. The extracts were cleaned up with MIP SPE cartridges. The separation was performed on a zwitter ionic-HILIC column (50 × 2.1 mm, 3.5 μm), with the mobile phase consisting of methanol, 0.3% formic acid, and 175 mmol/L ammonium formate at 0.50 mL/min in gradient elution. A triple-quadrupole mass spectrometer equipped with an electrospray ionization source, which was operated in positive mode, was used for detection. The quantification was based on matrix-matched calibration curves. The method was applied to real samples with three different matrixes. The LODs of the method were 2–30 μg/kg and the LOQs were 7–100 μg/kg; the average recovery ranged from 78.2 to 94.8%; intraday RSDs and interday RSDs were ≤15 and ≤18%, respectively; and the absolute values of matrix effect for all AGs were RSDs ≤23%.


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