scholarly journals SIMPLE ANALYTICAL METHOD FOR THE SIMULTANEOUS ESTIMATION OF HYDROCHLOROTHIAZIDE AND CANDESARTAN BY RP-HPLC

2017 ◽  
Vol 9 (6) ◽  
pp. 34
Author(s):  
Madhavi K. ◽  
Navamani M. ◽  
Prasanthi C.

Objective: To develop a simple, rapid, economic, accurate and precise reverse phase-high performance liquid chromatographic (RP-HPLC) method for the determination of hydrochlorothiazide and candesartan in the pharmaceutical dosage form and to validate as per international conference on harmonization (ICH) guidelines.Methods: The chromatographic separation was performed on Silanol BDS C18 column (250 x 4.6 mm, 5 μm), a mobile phase consisting of water (pH adjusted to 2.8 with orthophosphoric acid): acetonitrile (30:70 % v/v), with a flow rate 1 ml/min and the detection wavelength of 210 nm using photodiode array (PDA) detector.Results: The developed method resulted in elution of hydrochlorothiazide at 2.28 min and candesartan at 4.28 min. The calibration curves were linear (r2=0.999) in the concentration range of 6.25-18.75 μg/ml and 8-24 μg/ml for hydrochlorothiazide and candesartan respectively. The percentage recoveries were found to be 99.78-100.39 for hydrochlorothiazide and 99.87-100.64 for candesartan. The limit of detection (LOD) was found to be 0.410 μg/ml and 0.699 μg/ml for hydrochlorothiazide and candesartan respectively. The limit of quantitation (LOQ) was found to be 1.367 μg/ml and 2.330 μg/ml for hydrochlorothiazide and candesartan respectively.Conclusion: A simple, economic, accurate, precise, linear and rapid RP-HPLC method was developed for simultaneous quantitative estimation of hydrochlorothiazide and candesartan in bulk and pharmaceutical formulation and the method was validated as per ICH guidelines. Hence, the method holds good for the routine analysis of hydrochlorothiazide and candesartan in various pharmaceutical industries as well as in academics.

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 ◽  
2012 ◽  
Vol 49 (09) ◽  
pp. 27-32
Author(s):  
V. S Reddy ◽  
◽  
T. E. G. K. Murthy ◽  
N Usha Rani ◽  
R. S Rao ◽  
...  

A simple, precise, accurate, reproducible, robust reverse phase high-performance liquid chromatographic method was developed for the simultaneous estimation of frovatriptan, almotriptan and zolmitriptan in bulk and pharmaceutical dosage forms. The method was validated as per ICH and FDA guidelines. Analysis of the drugs was performed on Phenomenex Chromosil C-18 (250 x 4.6 mm, 5 mc) column, in an isocratic mode employing methanol, acetonitrile and THF in the ratio of 46:50:04 (v/v/v) as mobile phase. UV-visible detector at 269 nm was found to be suitable for detection. Linearity was observed in the range of 40-100 ppm.The % recovery was found to be 99.51, 99.69 and 99.34 for frovatriptan, almotriptan and zolmitriptan respectively. The % RSD values for method precision was found to be 0.86, 0.65 and 1.28 for frovatriptan, almotriptan and zolmitriptan respectively. Limit of quantification (LOQ) and limit of detection (LOD) values were found to be 0.15, 0.08 and 0.09 ppm. and 0.05, 0.02, 0.03 for frovatriptan, almotriptan and zolmitriptan respectively.


2012 ◽  
Vol 10 (2) ◽  
pp. 67-70
Author(s):  
Abdullah Al Masud ◽  
Mohammad Saydur Rahman ◽  
Towfika Islam ◽  
Saki Sultana ◽  
Moynul Hasan ◽  
...  

A simple, reproducible and efficient reversed phase high performance liquid chromatographic (RPHPLC) method has been developed for the estimation of a recently approved anti allergic drug, amlexanox in oral paste dosage form. The separations were carried out on a Zorbax Eclipse XBD, C18 column (150 x 4.6 mm; 5?m) at a flow rate of 1.50 ml/min. by using mobile phase comprising of mixed buffer (pH adjusted to 6.50) and methanol (50:50 v/v). The injection volume was 10 ?l and the peaks were detected at 244 nm. The linear dynamic range found to be in the concentration range of 15-35 ?g/ml and coefficient of correlation was found to be 0.999. The %RSD value was below 2.0 for intra-day and inter-day precision which indicated that the method was highly precise. The LOD (Limit of detection) and LOQ (Limit of quantitation) were found to be 3.8 ng/ml and 12.5 ng/ml, respectively which revealed that the method was highly sensitive. The percentage recovery of amlexanox ranged from 99.31 to 99.75%, indicating the accuracy of the method and absence of interference from the excipients present in the formulation. The proposed method was simple, fast, accurate and reproducible and hence can be applied for routine quality control operations of amlexanox in oral paste dosage form. Key words: Amlexanox, Anti allergic, RP-HPLC, LOD, LOQ. DOI: http://dx.doi.org/10.3329/dujps.v10i2.11782 Dhaka Univ. J. Pharm. Sci. 10(2): 67-70, 2011 (December)


2018 ◽  
Vol 10 (4) ◽  
pp. 111 ◽  
Author(s):  
Vandana Jain ◽  
Sultana Shaikh

Objective: To develop a novel, accurate, precise and linear reverse phase high performance liquid chromatographic (RP-HPLC) method for simultaneous qualitative and quantitative estimation of ellagic acid and quercetin in an ayurvedic formulation and validate as per international conference on harmonization (ICH) guidelines.Methods: In the present work, good chromatographic separation was achieved isocratically using a shim-pack HPLC C18 column (4.6 x 250 mm, 5μm) and a mobile phase consisting of 0.02 M potassium dihydrogen orthophosphate buffer (pH adjusted to 3.5 with orthophosphoric acid) and acetonitrile in the ratio 60:40, at flow rate of 1.2 ml/min and column temperature maintained at 35 °C. The effluents obtained were monitored at 255 nm with UV-visible detector.Results: The retention time of ellagic acid and quercetin were found to be 1.65 min and 2.94 min respectively. Linearity of ellagic acid and quercetin were tested in the range of 6-14 ppm and 3-11 ppm respectively. The correlation coefficient for ellagic acid and quercetin were 0.997 and 0.993 respectively. The high recovery values (98 %-102 %) indicate a satisfactory accuracy. The low percent relative standard deviation (% RSD) values in the precision study reveals that the method is precise.Conclusion: The developed method is novel, simple, precise, rapid, accurate and reproducible for simultaneous quantitative estimation of ellagic acid and quercetin in an ayurvedic formulation. Hence the developed method can be used for quantitative analysis and quality control of extracts and commercial samples of other plant species and formulation containing these two markers.


2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
S. Sowjanya ◽  
Ch. Devadasu

A reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed and validated for simultaneous estimation of levamisole and albendazole in drug substance and in its combinational dosage form. The analysis was carried out usingInertsil ODSC18(4.6 x 150 mm, 5μm) column, and the separation was carried out using a mobile phase containing a buffer of pH 3.5 and acetonitrile (70:30 v/v) pumped at a flow rate of 1.0 mL/min with variable wavelength UV-detection at 224 nm. Both the drugs were well resolved in the stationary phase and the retention times were 2.350 min and 4.055 for levamisole and albendazole, respectively. The method was validated and shown to be linear in the concentration range of 15-45μg/ml and 40-120μg/ml for levamisole and albendazole, respectively. The limit of detection (LOD) and limit of quantification (LOQ) were determined based on standard deviation of the y-intercept and the slope of the calibration curve. LOD and LOQ values were 2.08μg/ml and 6.03μg/ml for levamisole and 3.15μg/ml and 10.40μg/ml for albendazole, respectively. The accuracy of the method was assessed by adding known amount of standard solution (75 %, 100 %, and 125% of the sample concentration) to the preanalyzed sample solution of 100% concentration. All the samples were prepared and analyzed in triplicate. The percentage mean recovery by standard addition experiments of levamisole and albendazole is 99.66% and 98.73%, respectively.


Author(s):  
MADHAVI KUCHANA ◽  
CHAMUNDESWARI KANDUKURU ◽  
PRASANTHI CHENGALVA

Objective: To develop and validate a reverse phase high performance liquid chromatographic method for simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on reverse phase Discovery Inertsil ODS3V Column, C18 (250 mm, 4.6 mm, 5 µm). The separation was achieved by employing the mobile phase consists of phosphate buffer (pH 4) and acetonitrile (40:60). The flow rate was 1.0 ml/min, at a detection wavelength of 295 nm. The proposed method was validated as per the International Council for Harmonisation (ICH) guidelines.Results: The retention time for ciprofloxacin and fluocinolone acetonide was found at 3.627 min and 5.037 min respectively. The proposed method was validated for specificity, accuracy, precision, linearity, the limit of detection (LOD), limit of quantitation (LOQ) and robustness. All validation parameters were within the acceptable range. The assay method was linear and found in the range from 12.5–37.25 µg/ml for ciprofloxacin and 0.625–1.875 µg/ml of fluocinolone acetonide. The relative standard deviation (RSD) values for ciprofloxacin and fluocinolone acetonide were 0.25 % and 0.18 %, respectively. Conclusion: A rapid, accurate and precise RP-HPLC method was developed for the simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and ointment formulation. The developed method was validated for specificity, accuracy, precision, linearity, the limit of detection, limit of quantitation and robustness according to ICH guidelines.


Author(s):  
Darshan Bhatt ◽  
Padmini Thatavarthi ◽  
B. Rajkamal

A simple and sensitive reverse phase high performance liquid chromatographic method was developed and successively validated for the estimation of Canagliflozin. In the new method, Canagliflozin separation was carried out by the nonpolar inertsil ODS-3 (250 × 4.6 mm, 5μ) column with a mobile phase composition of Ammonium acetate buffer (pH-4.5) and Acetonitrile in the ratio of 30:70% v/v. Canagliflozin was determined at 252 nm using UV detection and the compound was eluted at the retention time of 4.5 min. As per International Conference on Harmonization (ICH) guidelines, the method was validated and the parameters were precision, accuracy, linearity, limit of detection, limit of quantitation and robustness. The chromatographic method was accurate, linear, specific, precise and robust. The results of method concluded that the proposed RP-HPLC method is useful, convenient and reliable in regular analysis of Canagliflozin in bulk and its formulation


Author(s):  
Vandana Jain ◽  
Revati Sonone ◽  
Leena Tandel

The objective of this paper was to develop and validate a novel, simple, rapid, precise and accurate, reverse-phase high-performance liquid chromatographic (RP-HPLC) method for simultaneous quantitative estimation of piperine and embelin in the herbal formulation as per the International Conference on Harmonization guidelines (ICH). Chromatographic separation was achieved using a Cosmosil C-18 (250*4.6mm) SH 5.0 µm column with a mobile phase consisting of methanol and 0.02 M phosphate buffer in ratio 98:2 v/v, (pH adjusted to 2.3 with ortho-phosphoric acid) at a flow rate of 1 mL/min and column temperature maintained at 28°C and ultraviolet (UV) detection at 288 nm. The retention time of piperine and embelin was found to be 4.15 and 5.69 min respectively. The linearity of piperine and embelin was tested in the range of 5-40 ?g/mL. The correlation coefficient for piperine and embelin was found to be 0.997 and 0.995, respectively. The recovery values (98-102%) indicate a satisfactory accuracy. The method was found to be precise as the percentage relative standard deviation was found to be <2 %. The proposed novel isocratic RP-HPLC method is rapid (short run time below 10 min), precise, accurate and sensitive. The method was successfully applied for the simultaneous analysis of piperine and embelin in herbal formulation.


2018 ◽  
Vol 10 (4) ◽  
pp. 51
Author(s):  
Pranay Wal ◽  
Ruchi Tiwari ◽  
Ankita Wal ◽  
Gaurav Tiwari

Objective: A fast, specific, and sensitive high-performance liquid chromatographic method has been developed and validated for the quantitative determination of unchanged Ramipril (RAM) and Telmisartan (TEL) in animal plasma.Methods: Analytes were extracted from animal plasma, 250 µl of animal plasma sample were mixed with internal working standard (25 ngmL-1) with the further addition of chloroform (HPLC Grade, Merck). The clear organic layer was separated and reconstituted to 1 ml in mobile phase and analysed by HPLC. The method was validated and evaluated in terms of linearity, accuracy, precision, specificity, limit of detection and limit of quantitation.Results: Absorption maxima of TEL and RAM was found to be 270 and 273 nm respectively. TEL and RAM with their respective internal standards (I. S.) were found to be well separated from the co-eluted components and there were no interferences from the endogenous material. The limit of detection (LOD) and limit of quantitation (LOQ) were found to be 2.01±.05; 4.88±0.10 and 0.11 and 0.25 for TEL and RAM respectively on the basis of a signal to noise ratio. The ruggedness of the method at various parameters was found to be±1.94% and±1.02% for TEL and RAM respectively. The low values of %RSD (<2.0) for each of the drug proposed that during all deliberate variations, middle-quality control (MQC) was not affected and it was in accordance with that of actual.Conclusion: Thus developed High-Performance Liquid Chromatography (HPLC) method was found to be more accurate, precise, sensitive, selective and reproducible.


Author(s):  
Venisetty R K ◽  
Kamarapu S K ◽  
Vaijayanthi ◽  
Bahlul ZEA

A simple, sensitive isocratic and reproducible reversed phase High Performance Liquid Chromatographic (RP-HPLC) method was developed for the estimation of ambroxol hydrochloride (ABH) and levocetirizine dihydrochloride (LCD) in combination using PDA detector. The system consisted of RP-C18 column and the detection was performed at 230nm. The mobile phase was a mixture of acetonitrile : phosphate buffer solution (60:40) (pH  7.0) pumped at room temperature and a flow rate of 1 ml/min. ABH and LCD were eluted at 2.75 and 5.01 sec respectively. The mean absolute recoveries of ABH and LCD were about 98 % and 99 % respectively and the limit of detection of LCD and ABH in the mixture of given proportion is observed to be 0.1 µg/ml and 1.5 µg/ml and the limit of quantitation is 0.3 µg/ml and 4.5 µg/ml respectively. The calibration was linear over a concentration range of 4.5 µg/ml to 15.0 µg/ml with r2 > 0.997 for ABH and 0.3 µg/ml to 1.0 µg/ml with r2 > 0.999 for LCD. The intra (n = 5) and inter (n = 5) day assay variations in the linear range are < 4 % for ABH and < 6 % for LCD. Three pharmaceutical products containing this combination are analyzed to test the applicability of the new method. The percentage of ABH and LCD in three marketed capsule dosage form studied range from 99 to 102 % and 100 to 103 % and respectively to the claimed value.


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