scholarly journals A Novel Synchronic Estimstion of Metronidazole, Ciprofloxacin and Doxycycline by RP-HPLC in Bulk and Pharmaceutical Formulation

Author(s):  
Rama Rao Nadendla ◽  
Siva Prasad Morla ◽  
Abhinandana Patchala ◽  
Prachet Pinnamaneni

Aim: To design simple, rapid, new analytical method for estimation of Metronidazole, Ciprofloxacin Doxycycline by using RP-HPLC in bulk and pharmaceutical dosage form. Study Design: Estimation of Metronidazole, Ciprofloxacin Doxycycline by using RP-HPLC in bulk and pharmaceutical dosage form was planned and executed. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute Of Pharmaceutical Sciences, Lam, Guntur-522034, Andhra Pradesh, India during the period of November 2019 to February 2020. Methodology: Metronidazole is an antibiotic and antiprotozoal medication. It is used either alone or with other antibiotics to treat pelvic inflammatory disease, endocarditis and bacterial vaginosis. Ciprofloxacin is an antibiotic used to treat a number of bacterial infections. Doxycycline is a tetracycline antibiotic that fights bacteria in the body. The study was carried out on SHIMADZU Prominance-i, LC-2030C system equipped with Shim-pack Gist (250 x 4.6 mm, 5μm) column and mobile phase was optimized by using mixture of methanol and 0.25mM potassium phosphate buffer in the ration of 60:40 v/v at a flow rate of 0.8 ml/min. The wavelength was set as 282nm at ambient temperature by injecting 20µl of solution and the run time was fixed for 10 min. Results: Linearity plot was constructed for concentration range of 5-15µg/ml for Metronidazole,5-15µg/ml for Ciprofloxacin and 1-8µg/ml for Doxycycline standard solutions. It shows best regression coefficient and y/s values. The accuracy of the proposed method was determined by performing recovery studies and was found between 98-102%. The repeatability testing for both sample and standard solutions the %RSD was found as <2.0% which is within the acceptable limits showing that the method is precise as well. The LOD and LOQ were found to be 0.33 and 0.99 µg/ml for Metronidazole, 0.33 and 0.99 µg/ml for Ciprofloxacin, 0.08 and 0.25 µg/ml for Doxycycline respectively. The proposed method was successfully applied for the pharmaceutical dosage form of Metronidazole, Ciprofloxacin Doxycycline and it was as economic, eco-friendly with less retention time around 10.0 min. Conclusion: The proposed method was validated in terms of linearity, range, Accuracy, precision, Specificity, Robustness. Method was successfully applied to the estimation of Metronidazole, Ciprofloxacin Doxycycline in combined marketed pharmaceutical dosage form.

Author(s):  
Rama Rao Nadendla ◽  
Patchala Abhinandana

Aim: The main aim of the current study is to give best and simple method for the estimation of antiparkinsonian drugs named Carbidopa, levodopa and entacapone. Study Design:  Simultaneous estimation of Carbidopa, levodopa and entacapone was performed by using Quadrapumped (SHIMADZU Prominance-i, LC-2030C) RP-HPLC equipped with PDA detector. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute Of Pharmaceutical Sciences, Lam, Guntur-522034, Andhra Pradesh, India during the period of August 2019 to February 2020. Methodology: The assets of the study can determined as the process of qualification and quantification was done on SHIMADZU Prominance-i, LC-2030C system equipped with Phenomenex ODS (150 x 4.6 mm, 5μm) column and mobile phase was optimized using combination of acetonitrile and 0.1% ortho phosphoric acid in the ration of 50:50 v/v at a flow rate 1.0 ml/min. The wavelength was set as 270nm at ambient temperature by injecting 20µl of solution and the run time was fixed for 5 min. Results: Calibration plot shown best regression over the concentration range of 5-160 µg/ml of Carbidopa, Levodopa and Entacapone standard solutions. The LOD and LOQ were found to be 0.85 and 2.54 µg/ml for Entacapone, 0.24 and 0.71 µg/ml for Levodopa, 0.14 and 0.43 µg/ml for Carbidopa respectively. The accuracy of the proposed method was determined by performing recovery studies and was found to be between 98-102%. The repeatability testing for both sample and standard solutions was found as %RSD<2.0% which is within the acceptable limits showing that the method is precise as well. The proposed method was successfully applied for the marketed formulations of Carbidopa, Levodopa and Entacapone tablets. In addition the main feature of proposed method is economic and eco-friendly with less retention time around 5.0 min. Conclusion: Including all the optimized method parameters and statistical results given it can be concluded as a new, simple, sensitive, precise and accurate economical analytical method was developed and validated by RP-HPLC for the detection and quantification of Carbidopa, Levodopa and Entacapone which can be applied to the marketed formulation where there are no official compendial methods reported for this particular combination. The high sensitivity (LOD), mobile phase utilized and run time (=5) can be determined as an important features for this proposal.


Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.


INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (12) ◽  
pp. 32-36
Author(s):  
T. Vishalakhi ◽  
◽  
S. K Kumar ◽  
K Sujana ◽  
P Rani

A simple validated RP HPLC method for the estimation of rizatriptan benzoate in pharmaceutical dosage form and bulk was developed for routine analysis. This method was developed by selecting Agilent TC C18 (250 x 4.6 mm, 5 μ) column as stationary phase and acrylonibrile:water (45:55), pH adjusted to 3, as mobile phase. Flow rate of mobile phase was maintained at 4: 1 mL/min at ambient temperature throughout the experiment. Quantification was achieved with ultraviolet (DAD) detection at 220 nm. The retention time obtained for rizatriptan was 2.8 min. The detector response was linear in the concentration range of 2-25μg/mL. This method was validated and shown to be specific, sensitive, precise, linear, accurate, rugged and robust. Hence, this method can be applied for routine quality control of rizatriptan benzoate in dosage forms as well as in bulk drug.


Author(s):  
G.M. Kadam ◽  
A.L. Puyad ◽  
T.M. Kalyankar

A new, economical, simple, accurate, and precise RP-HPLC method was developed for simultaneous assay and content uniformity determination of Sacubitril and Valsartan in bulk and pharmaceutical dosage form. The separation of Sacubitril and Valsartan was achieved within 6 minutes on Phenomenex Luna C18 250 mm x 4.6mm and 5µm Particle Size, column using Acetonitrile: Methanol: Water (30:55:15% v/v/v) as the mobile phase. Detection was carried out at 250 nm wavelength. The retention time of Sacubitril and Valsartan was found to be 2.361 and 3.304 min, respectively. The validation of the developed method was performed in terms of specificity, accuracy, precision, linearity, the limit of detection, the limit of quantification as mentioned in International Conference on Harmonization (ICH) guidelines. The method showed adequate sensitivity concerning linearity, accuracy, and precision over the range 12-36 μg/ml and 13-39 μg/ml for Sacubitril and Valsartan, respectively. The percentage recoveries obtained for Sacubitril and Valsartan were found to be in the range of 98.00 – 102.00 %. The proposed method is suitable for use in quality-control laboratories for quantitative analysis.


2011 ◽  
Vol 34 (18) ◽  
pp. 2185-2195 ◽  
Author(s):  
Sharmistha Mohapatra ◽  
M. Mathrusri Annapurna ◽  
B. V. V. Ravi Kumar ◽  
Mohammed Anwar ◽  
Musarrat Husain Warsi ◽  
...  

Author(s):  
Ch. Jaswanth Kumar ◽  
Prachet Pinnamaneni ◽  
Siva Prasad Morla ◽  
K. N. Rajini Kanth ◽  
Rama Rao Nadendla

Aims: The main aim of the present study was to develop and validate a simple and cost- effective method for the estimation of allopurinol and its related substances by using RP-HPLC. Study Design:  Estimation of Allopurinol and its related substance in bulk and tablet dosage forms by RP-HPLC. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute of Pharmaceutical Sciences, Chalapathi Nagar, Lam, Guntur-522034 between October 2020 to January 2021. Methodology: Method development was carried out by using Schimadzu, Prominence-i series LC 3D-Plus autosampler embedded with lab solutions software, equipped with PDA detector using YMC column (150 mm X 4.6 mm, 3 μm) and 0.1M Ammonium acetate buffer as a mobile phase in the ratio of 100% at a flow rate of 1.0 ml/min at a wavelength of 255nm. The developed method was validated according to ICH guidelines. Results:  The linearity was observed in the range of 20-100 µg/ml with a regression (R2) value of 0.999. Developed method was specific with no interactions and accurate with 100.11% for allopurinol and 99.54% for its related substance. The limit of detection for allopurinol was 2 µg/ml and for related substance was 0.0.1 µg/ml. The limit of quantification for allopurinol was 6 µg/ml and for related substance was 0.03 µg/ml respectively. The percentage relative standard deviation was found to be NMT 2 which indicates that the proposed method was precise and robust. Conclusion:  The developed method was simple, precise and accurate and can be successfully employed for the estimation of allopurinol in bulk and tablet dosage form.


Author(s):  
Sireesha D ◽  
Sai Lakshmi E ◽  
Sravya E ◽  
Vasudha Bakshi

A new simple, rapid, specific, accurate, precise and novel Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method has been developed for the estimation of Sitagliptin Phosphate in the pharmaceutical dosage form. The chromatographic separation for Sitagliptin was achieved with mobile phase containing methanol, Thermoscientific C18 column, (250x4.6 particle size of 5μ) at room temperature and UV detection at 248 nm. The compounds were eluted in the isocratic mode at a flow rate of 1ml/min. The retention time of Sitagliptin was 1.91min. The above method was validated in terms of linearity, accuracy, precision, LOD and LOQ in accordance with ICH guidelines.


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