scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF CURCUMIN AND PIPERINE BY RP-HPLC

2019 ◽  
Vol 11 (1) ◽  
pp. 216 ◽  
Author(s):  
Ramya Kuber B.

Objective: To develop a simple, sensitive, specific, accurate reverse phase high performance liquid chromatographic (RP-HPLC) method for the estimation of curcumin and piperine.Methods: The separation was done using a column Inertsil–ODS C18 (250 mm × 4.6 mm, 5µ particle size) and mobile phase composed of methanol: water (45:55 v/v), flow rate at 1 ml/min and detection was carried out at 282 nm with photodiode array (PDA) detector.Results: The separation of curcumin and piperine were found to be at the retention time of 2.433 min and 3.095 min, respectively. The method was found to be linear at a concentration range 20-80 µg/ml for curcumin and piperine. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.05µg/ml and 0.17µg/ml for curcumin and 0.18µg/ml and 0.53µg/ml for piperine respectively. The average percentage recoveries of curcumin and piperine were in the range of 98-100.6%.Conclusion: A simple and sensitive reverse phase high performance liquid chromatographic method was developed for the estimation of curcumin and piperine.

Author(s):  
Sunkara Namratha ◽  
Vijayalakshmi A

Objective: Reversed-phase high-performance liquid chromatographic method (RP-HPLC) was developed for the assessment of lopinavir in the dosage form of tablet.Methods: Chromatogram was run through using Kromosil C18 4.5×150 mm using a mobile phase methanol: water of ratio 65:35% v/v with a rate of flow of 0.8 ml/min, measured by UV spectrometric detection at 265 nm. The method developed was validated in terms of precision, accuracy, linearity, and robustness parameters.Results: Retention time of lopinavir established at 2.482 min and percentage R.S.D of lopinavir found to be 1.0% and 0.5%, respectively. The method shows that good linearity range of 30–150 μg correlation coefficient of lopinavir was 0.997. The limit of detection was 2.97 and limit of quantification was 9.92, respectively. The percent purity of lopinavir was 99.87%.Conclusion: The suggested method (Rp-HPLC) for concurrent assay lopinavir was validated, which is appropriate method for the analysis oflopinavir quantitatively in tablet dosage forms and bulk.


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.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 76-78
Author(s):  
Kailasa Mangasree ◽  
◽  
Biswabara Roy ◽  
Harunrasheed Shaik ◽  
Manjunath S. Yalagatti ◽  
...  

A reverse phase high performance liquid chromatographic method was developed for simultaneous estimation of gemcitabine and clarithromycin in bulk and tablet dosage form. The method was developed by using acetonitrile: methanol: 50 mM sodium acetate buffer (adjusted to pH-3 with orthophosphoric acid (40:40:20) as a mobile phase at the flow rate of 1mL/min. The retention time was found to be 2.365 and 5.999 minutes, respectively. The method showed linearity in the concentration range 10-50 µg/mL in respect of both drugs. The % RSD was less than 0.4% for gemcitabine and 0.2% for clarithromycin. Mean percentage recovery was found to be 99.63 and 99.69 for gemcitabine and clarithromycin. The tailing factor for gemcitabine and clarithromycin was not less than 0.9 and not more than 1.4 during the robustness study. The average percentage assay was calculated and found to be 99.83 for gemcitabine and 98.89 for charithromycin. The limit of detection and quantification for gemcitabine was found to be 0.41 and 1.79 µg/mL. For Clarithromycin, the value was 0.58 and 1.37 µg/mL respectively.


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


2020 ◽  
Vol 58 (8) ◽  
pp. 695-699
Author(s):  
Muhammad Asad Saeed ◽  
Muhammad Tayyab Ansari ◽  
Bashir Ahmad Ch ◽  
Muhammad Zaman

Abstract A simple, rapid and cost-effective reverse phase high-performance liquid chromatographic (RP-HPLC) method was developed for the quantification of artesunate. C18 Promosil (ODS, 150 × 4.6 mm, 5 μm) column was used as stationary phase to separate the drug. Mobile phase comprised of ethanol: water (65:35) having pH 4.5 was run isocratically at a flow rate of 1 mL/min at 27°C. The method was validated according to ICH guidelines for linearity, precision, accuracy, robustness, specificity, limit of detection (LOD) and limit of quantification (LOQ). The method was found accurate, precise and robust with an average retention time of 4.509 min and 0.5357 %RSD. Good linearity was observed in the concentration range of 2–10 mg/ml with regression coefficient R2 value of 0.9995 and slope value of 369,928. Conclusively, as per ICH norms, the developed method was successfully validated and used for the quantification of artesunate in fast dissolving tablets (FDTs).


2020 ◽  
Vol 21 (2) ◽  
pp. 247-253
Author(s):  
Salman Khurshid

A precise, accurate, simple and low cost reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the simultaneous quality assessment of commonly used insecticide carbofuran and fipronil in its technical and formulated products. The chromatographic parameters, i.e. mobile phase composition, wavelength and flow rate of developed method was optimized in such a way that the HPLC was carried out at 280 nm by using a mobile phase, which contains 80 parts acetonitrile and 20 parts water by volume (ACN:H2O, 80:20) flowing at a rate of 1.0 mL/min. A linear relationship (R2 > 0.999) was shown by calibration curve plotted in the concentration ranged from 30-800 mg/L. The limit of detection (LODs) were found to be 14.5 mg/L and 20.9 mg/L and limit of quantification (LOQs) were recorded to be 43.9 mg/L and 63.2 mg/L for both carbofuran and fipronil respectively. The developed method’s accuracy was exhibited by recovery percentage (96.0-100.8) % of water samples spiked with 100, 300 and 600 mg/L of carbofuran and fipronil, respectively. The developed RP-HPLC method is therefore simple, cheap, rapid and can be proficiently used for the simultaneous identification and quantification of carbofuran and fipronil in its technical and formulated products.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.


Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.


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.


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