scholarly journals Stability indicating RP-HPLC method development and validation for the simultaneous estimation of ceftriaxone and tazobactum in sterile powder for injection

T. Vimalakkannan ◽  
P. Shaik Parveen ◽  
Salomi ◽  
K. Ravindra Reddy

A simple, rapid, precise and accurate method is developed for the quantitative simultaneous determination of ceftriaxone and tazobactum in bulk and pharmaceutical formulations. Separation of ceftriaxone and tazobactum was successfully achieved by using Inertsil C18 ODS column 250X4.6mm, 5µm in an isocratic mode using water and acetonitrile (80:20) at a flow rate of 1.0 ml/min and was monitored at 254 nm with a retention time of 3.049 minutes and 4.317 minutes for ceftriaxone and tazobactum respectively. The method was validated and the response was found to be linear in the drug concentration range of 20µg/ml to 80 µg/ml for ceftriaxone and 5 µg/ml to 35 µg/ml for tazobactum. The values of the correlation coefficient were found to be 0.999 for ceftriaxone and 0.999 for tazobactum respectively. The LOD and LOQ for ceftriaxone were found to be 0.021 and 0.064 respectively. The LOD and LOQ for tazobactum were found to be 0.030 and 0.091 respectively. The percentage recovery for ceftriaxone and tazobactum were found to be 98-102% respectively which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.  Stability of the drugs was determined by using acid/base, thermal, oxidative stress testing.

2010 ◽  
Vol 5 (4) ◽  
pp. 1934578X1000500 ◽  
Raju Gautam ◽  
Amit Srivastava ◽  
Sanjay M. Jachak

An HPLC method with reflux as an efficient extraction method has been developed for quantification of chromones in Dysophylla stellata Benth. Separation was achieved on a C18 column with a mobile phase of 0.5% (v/v) acetic acid in water (A), and ACN (B) under gradient elution at 1 mL/min. Chromones (1 and 2) isolated from D. stellata were used as standards for method development and validation was achieved according to ICH guidelines. Extracts prepared by three different methods [reflux, ultrasonication and accelerated solvent extraction (ASE)] were used for analysis by the validated method. The proposed HPLC method is simple, accurate and selective for the separation and quantification of chromones in D. stellata.

2019 ◽  
Vol 10 (2) ◽  
pp. 113-117
Elham Anwar Taha ◽  
Manal Mohammed Fouad ◽  
Ali Kamal Attia ◽  
Zainab Mahmoud Yousef

A rapid and sensitive High Performance Liquid Chromatography (HPLC) method has been developed and validated as per ICH guideline for simultaneous determination of ramipril and felodipine binary mixture. Chromatographic separation was achieved on a Hyperchom C18 column (250 × 4.6 mm i.d., 5 μm) using an isocratic mobile phase of potassium di-hydrogen phosphate (pH = 3.4): methanol: acetonitrile in the ratio 15:15:70 (v:v:v). The flow rate was 1.5 mL/min, temperature of the column was maintained at 30 °C and detection was made at 210 nm. Linearity studies indicated that the drugs obey Beer’s law over the range of 10-80 μg/mL for ramipril and 5-80 μg/mL for felodipine. The proposed method is precise, accurate, linear and robust. The short retention time allows the analysis of a large number of samples in a short period of time and, therefore, considered to be cost-effective that can be used for routine analysis of both drugs in the pharmaceutical industry.

2019 ◽  
Vol 10 (04) ◽  
pp. 583-587
Venkata Nanda Kumar Kopparapu ◽  
Poornima Kasula ◽  
Ajay Kumar Reddy Ankinapalli ◽  
M Venkateswarlu

Paracetamol (PCT) and Mefenamic acid (MFA), in combination, is recommended widely for the treatment of antipyretic and anti-inflammatory conditions. The present works carry a new simple, rapid, precise, accurate, and sensitized method of high-performance liquid chromatography with UV detection for simultaneous quantification of PCT and MFA. The samples are eluted in isocratic mode using a Phenomenex ODS 3V C18 (4.6mm × 250 mm i.d, with a particle size of 5μm) with the mobile composition of methanol: phosphate buffer pH 7.1 (70:30) delivered at a flow rate of 1ml/min with the detection wavelength of 254 nm. It shows good linearity response in the concentration range of 15-35 μg/mL and 6-14 μg/ml for PCT and MFA with the retention times of 3.0 min and 4.8 min, respectively. The quantities of PCT and MFA in pharmaceutical suspension were found to be 99.01% and 101.02%, respectively. The method was quantitatively evaluated according to ICH guidelines taking into consideration the required parameters, and the results obtained are within acceptable limits. So, the proposed method can be employed in the routine analysis and evaluation of MFA and PCT in both bulk and suspension dosage form.

Ankita Shinde ◽  
G.B. Gajeli ◽  
Sneha Ubale ◽  
Vinod Matole

A new, simple, rapid, selective, precise and accurate reverse phase high performance liquid chromatography assay has been developed for simultaneous estimation of Bilastine, and Montelukast in tablet formulations. The separation was achieved by using Phenomenax Kinetex XB C-18 column (150 x 4.6mm, 5 .) using mobile phase Methanol: 0.1% TFA water (80:20). Injection volume was 10µl. The flow rate was 1.0mL.min-1 and the separated drugs were detected using UV detector at the wavelength of 270nm. The retention time of Bilastine and Montelukast was noted to be 1.27, and 4.86 respectively, indicative of rather shorter analysis time. The method was validated as per ICH guidelines. The proposed method was found to be accurate, reproducible, and consistent. It was successfully applied for the analysis of these drugs in marketed formulations and could be effectively used for the routine analysis of formulations containing any one of the above drugs, or a combination, without any alteration in the chromatographic conditions.

2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
L Mohankrishna ◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

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