scholarly journals Quantitative Estimation of Parthenolide in Tanacetum parthenium (L.) Schultz-Bip. Cultivated in Egypt

2007 ◽  
Vol 90 (1) ◽  
pp. 21-27 ◽  
Author(s):  
Ali M El-Shamy ◽  
Seham S El-Hawary ◽  
Mostafa E M Rateb

Abstract Parthenolide, a germacranolide-type sesquiterpene lactone, was estimated in Tanacetum parthenium (L.) cultivated in Egypt by using colorimetric, planar chromatographic, and high-performance liquid chromatographic (HPLC) methods. Parthenolide levels in the open-field herb and aseptically germinated shoots were also compared by using the HPLC method. Parthenolide was produced and estimated for the first time in the callus culture of the plant. In addition, 2 Egyptian market preparations were analyzed for their parthenolide content by using the HPLC method. The relative standard deviations were 0.093, 0.095, and 0.098% (n = 5,5,and 7, respectively), and the corresponding recoveries were 98.2, 98.9, and 99.4% for the colorimetric, planar chromatographic, and HPLC determinations, respectively.

Author(s):  
Sultana Shaikh ◽  
Vandana Jain

Objective: The objective of the study was 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, quercetin, and piperine in different Ayurvedic formulations and validate as per the International Conference on Harmonization guidelines. Methods: In the present work, a good chromatographic separation was achieved isocratically using a shim-pack HPLC C18 column (4.6×250 mm, 5 μm) 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, a flow rate of 1.2 ml/min and column temperature maintained at 35°C. The effluents obtained were monitored at 255 nm with ultraviolet-visible detector. Results: The retention time of ellagic acid, quercetin, and piperine was found to be 1.65 min, 2.94 min, and 14.57 min, respectively. The linearity of ellagic acid, quercetin, and piperine was tested in the range of 6–14 ppm, 3–11 ppm, and 3–13 ppm, respectively. The correlation coefficient for ellagic acid, quercetin, and piperine was found to be 0.997, 0.993, and 0.99, respectively. The high recovery values (98–102%) indicate a satisfactory accuracy. The low percent relative standard deviation values in the precision study reveal that the method is precise. Conclusion: The developed method is novel, simple, precise, rapid, accurate, and reproducible for simultaneous quantitative estimation of ellagic acid, quercetin, and piperine in Ayurvedic formulations. Hence, the developed method can be used for quantitative analysis and quality control of extracts and commercial samples of other plant species and formulations containing these three markers.


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.


Author(s):  
Sultana Shaikh ◽  
Vandana Jain

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 curcumin, piperine and camphor 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 mobile phase consisting of 0.02 M potassium dihydrogen orthophosphate buffer (pH adjusted to 3.5 with orthophosphoric acid) and acetonitrile in the ratio 40:60, at flow rate of 1 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 curcumin, piperine and camphor was found to be 6.57 min, 7.32 min and 8.57 min respectively. Linearity of curcumin and camphor were found in the range of 4-8 ppm and that of piperine was found to be 5-9 ppm. The correlation coefficient for curcumin, piperine and camphor were 0.998, 0.99 and 0.994 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 curcumin, piperine and camphor in an ayurvedic formulation. Hence the developed method can be used for quantitative analysis and quality control of extracts and commercial samples of other species containing these three markers.


2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.


2008 ◽  
Vol 91 (2) ◽  
pp. 387-391 ◽  
Author(s):  
Jaeho Ha ◽  
Kyu-Jai Han ◽  
Ki-Jin Kim ◽  
Seung-Weon Jeong

Abstract A sensitive, precise, and specific gas chromatographic (GC) method was developed for the analysis of capsaicin in Gochujang and validated by comparing with a column high-performance liquid chromatographic (HPLC) method (AOAC 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The GC separation was performed on a (5 phenyl)-methylpolysiloxane column [length 30 m, internal diameter (id) 250 μm, film thickness 0.25 μm] followed by flame ionization detection. The conditions of temperature programming were initially 220Cfor 1min, rampat5C/minto270C, and hold for 10 min. The recovery of capsaicin in Gochujang was more than 92, and the detection limit and lower determination limit of the GC analysis were 1.0 and 5.0 μg/g, respectively. The calibration graph for capsaicin was linear from 1 to 250 μg/mL for GC and 0.5 to 50 μg/mL for HPLC. The interday and intraday precisions (relative standard deviations) were <4.02.


1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.


2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Hong Yan ◽  
Pei Xu ◽  
Hai Huang ◽  
Juan Qiu

AbstractA pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.


1980 ◽  
Vol 63 (6) ◽  
pp. 1262-1265
Author(s):  
Edward R Townley ◽  
Bruce Ross

Abstract A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol–water–acetic acid (66+33+1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a µBondapak C18 column and methanol–water–acetic acid (66+33+1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate pairedion reagent. Average recovery is 98.7% with a relative standard deviation of ±2.3% for the equipment described.


2019 ◽  
Vol 16 (1) ◽  
pp. 12-23
Author(s):  
Nila Mary Varghese ◽  
Venkatachalam Senthil ◽  
Sajan Jose ◽  
Cinu Thomas ◽  
Jyoti Harindran

Objective: A simple, accurate and economical reverse phase- high performance liquid chromatographic method has been developed for the simultaneous quantitative estimation of two anti-retro viral drugs, Etravirine and Elvitegravir in nanoparticulate formulations for the first time. This method is a novel analytical technique for the detection of the both the drugs concurrently, as there is no method available for their simultaneous quantification, to the best of our knowledge. Methods: Optimization and validation of the chromatographic conditions were completed according to the standard ICH guidelines. The separation was done on a C18 column (250 mm x 4.6mm, 5μm) using methanol and phosphate buffer of pH (5.6) as the mobile phase in the ratio 78:22 v/v at a flow rate of 1ml/min for a short run time of 13 min. The detection wavelength was 285nm and the column temperature was maintained at 32oC. Results: The developed method was linear over 10 to 160 μg/ml with a regression coefficient of 0.999 for each. The LOD values were 4.83 and 9.25 µg/ml while LOQ values were 14.63 and 28.01 µg/ml for etravirine and elvitegravir respectively. The recovery values obtained by etravirine and elvitegravir were between 97.6% and 100.8%. Conclusion: The method was specific, precise, fast and accurate with good inter and intra day precision. The method was also effectively employed for the characterization and simultaneous quantification of both drugs in nanoparticulate formulation.


Author(s):  
Sv Saibaba ◽  
Shanmuga Pandiyan P

Objective: To develop and validate reverse phase-high performance liquid chromatographic method for estimation of olanzapine in bulk and tablet dosage form.Methods: Chromatographic analysis was performed on XTerra C18 (150×3.5 mm inner diameter, 5 μm) column using a mobile phase consisting of buffer (potassium dihydrogen phosphate) and methanol (45:55% v/v) with a flow rate of 0.6 ml/minutes. The detection was carried out at 247 nm.Results: The calibration curve of olanzapine was linear in the range of 30-70 μg/ml. The mean % assay of marketed formulation was found to be 100.2%, and % recovery was observed in the range of 98-102%. Relative standard deviation for the precision study was found <2%.Conclusion: The developed method is simple, precise and rapid, making it suitable for estimation of olanzapine in bulk and tablet dosage form.Keywords: Olanzapine, Reverse phase-high performance liquid chromatographic, Validation.


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