scholarly journals Developing a high-performance liquid chromatography fast and accurate method for quantification of silibinin

2019 ◽  
Vol 12 (1) ◽  
Author(s):  
Faezeh Bakhshi ◽  
Ommoleila Molavi ◽  
Mohammad Reza Rashidi ◽  
Ali Shayanfar ◽  
Hassan Amini

Abstract Objective Silibinin is an antioxidant agent and is shown to have anticancer effects in different cancers including lung, breast, colorectal, liver, prostate, and kidney. There are challenges in the clinical use of silibinin. The main limitation is low solubility, poor oral absorption, and extensive hepatic metabolism. We aim to develop a High-Performance Liquid Chromatography (HPLC) sensitive method for quantification of silibinin in aqueous samples to quantify its concentration in new formulations. A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase and the mixture of methanol (90%) and water (10%) as mobile phase. The developed method was validated based on the established guidelines. Results The retention time for silibinin was seen in 2.97 min after injection. The calibration curve was drawn and the established method demonstrated a linear ranged from 10 to 100 µg/ml, with a correlation coefficient of 0.996. The sensitivity of the developed method was 10 µg/ml. The accuracy calculated in the range of 88–105.9% and the precision (as relative standard deviation) was between 2.7 and 10.9%. These results demonstrate that the developed method can be a fast and accurate method for quantification of silibinin in aqueous samples.

2019 ◽  
Author(s):  
Faezeh Bakhshi ◽  
Ommoleila Molavi ◽  
Mohammad Reza Rashidi ◽  
Ali Shayanfar ◽  
Hassan Amini

Abstract Objective : Silibinin is an antioxidant agent and is shown to have anticancer effects in different cancers including lung, breast, colorectal, liver, prostate, and kidney. There are challenges in the clinical use of silibinin. The main limitation is low solubility, poor oral absorption, and extensive hepatic metabolism. We aim to develop a High-Performance Liquid Chromatography (HPLC) sensitive method for quantification of silibinin in aqueous samples to quantify its concentration in new formulations. A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase and the mixture of methanol (90%) and water (10%) as mobile phase. The developed method was validated based on the established guidelines. Results : The retention time for silibinin was seen in 2.97 minute after injection. The calibration curve was drawn and the established method demonstrated a linear ranged from 10 to 100 µg/ml, with a correlation coefficient of 0.996. The sensitivity of the developed method was 10 µg/ml. The accuracy calculated in the range of 88-105.9% and the precision (as relative standard deviation) was between 2.7-10.9%. These results demonstrate that the developed method can be a fast and accurate method for quantification of silibinin in aqueous samples.


2019 ◽  
Author(s):  
Faezeh Bakhshi ◽  
Ommoleila Molavi ◽  
Mohammad Reza Rashidi ◽  
Ali Shayanfar ◽  
Hassan Amini

Abstract Objective : Silibinin is an antioxidant agent and is shown to have anticancer effects in different cancers including lung, breast, colorectal, liver, prostate, and kidney. There are challenges in the clinical use of silibinin. The main limitation is low solubility, poor oral absorption, and extensive hepatic metabolism. We aim to develop a High-Performance Liquid Chromatography (HPLC) sensitive method for quantification of silibinin in aqueous samples to quantify its concentration in new formulations. A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase and the mixture of methanol (90%) and water (10%) as mobile phase. The developed method was validated based on the established guidelines. Results : The retention time for silibinin was seen in 2.97 minute after injection. The calibration curve was drawn and the established method demonstrated a linear ranged from 10 to 100 µg/ml, with a correlation coefficient of 0.996. The sensitivity of the developed method was 10 µg/ml. The accuracy calculated in the range of 88-105.9% and the precision (as relative standard deviation) was between 2.7-10.9%. These results demonstrate that the developed method can be a fast and accurate method for quantification of silibinin in aqueous samples.


2019 ◽  
Author(s):  
Faezeh Bakhshi ◽  
Ommoleila Molavi ◽  
Mohammad Reza Rashidi ◽  
Ali Shayanfar ◽  
Hassan Amini

Abstract Objective: Silibinin is an antioxidant agent and is shown to have anticancer effects in different cancers including lung, breast, colorectal, liver, prostate, and kidney. There are challenges in the clinical use of silibinin. The main limitation is low solubility, poor oral absorption, and extensive hepatic metabolism. We aim to develop a High-Performance Liquid Chromatography (HPLC) sensitive method for quantification of silibinin in in-vitro samples to quantify its concentration in new formulations. A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase and the mixture of methanol (90%) and water (10%) as mobile phase. The developed method was validated based on the established guidelines. Results: The retention time for silibinin was seen in 2.97 minute after injection. The calibration curve was drawn and the established method demonstrated a linear ranged from 10 to 100 µg/ml, with a correlation coefficient of 0.996. The sensitivity of the developed method was 10 µg/ml. The accuracy calculated in the range of 88-105.9% and the precision (as relative standard deviation) was between 2.7-10.9%. These results demonstrate that the developed method can be a fast and accurate method for quantification of silibinin in aqueous samples.


2019 ◽  
Author(s):  
Faezeh Bakhshi ◽  
Ommoleila Molavi ◽  
Mohammad Reza Rashidi ◽  
Ali Shayanfar ◽  
Hassan Amini

Abstract Objective : Silibinin is an antioxidant agent and is shown to have anticancer effects in different cancers including lung, breast, colorectal, liver, prostate, and kidney. There are challenges in the clinical use of Silibinin. The main limitation is low solubility, poor oral absorption, and extensive hepatic metabolism. We developed a High-Performance Liquid Chromatography sensitive method for quantification of Silibinin in in-vitro samples to quantify in different formulations. We applied HPLC set, C18 column as stationary phase and the mixture of methanol (90%) and water (10%) as mobile phase. Utilized solutions were daily prepared through serial dilution of stock solution to make specific concentrations ranged between 10 μg/ml to 100 μg/ml. The developed method was validated by credible guidelines. Results : The calibration curve was drawn according to the height peaks of different concentrations and the established method demonstrated a linear ranged from 10 to 100 µg/ml, with a correlation coefficient of 0.996 for in-vitro samples. The retention time was 2.97 min, and the accuracy and precision (inter-day and intra-day) of the developed method was in the range of 88-105.9%. These results demonstrate that the developed method can be a fast and accurate method for quantification of Silibinin in in-vitro samples.


2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.


2017 ◽  
Vol 2017 ◽  
pp. 1-7
Author(s):  
Paula Karina S. Uchoa ◽  
Leandro Bezerra de Lima ◽  
Antonia T. A. Pimenta ◽  
Maria da Conceição F. de Oliveira ◽  
Jair Mafezoli ◽  
...  

A high-performance liquid chromatography method was developed and validated for the quantification of the cytotoxic compounds produced by a marine strain ofAspergillus niger. The fungus was grown in malt peptone dextrose (MPD), potato dextrose yeast (PDY), and mannitol peptone yeast (MnPY) media during 7, 14, 21, and 28 days, and the natural products were identified by standard compounds. The validation parameters obtained were selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation below 5%), and accuracy (recovery > 96).


2012 ◽  
Vol 550-553 ◽  
pp. 1173-1176
Author(s):  
Hui Qing Sun ◽  
Yi Qiang Li ◽  
Guang Jun Xu ◽  
Xiao Zhen ◽  
Jin Li Xu ◽  
...  

Abstract. [Aims] A high performance liquid chromatography (HPLC) was presented for determination of fentin acetate residue in beet and soils. [Methods] Fentin acetate was extracted from beet plants and soils with hydrochloric acid and acetonitrile, followed by a second extraction in dichloromethane, purified by acid aluminium oxide with methanol eluting, then dissolved by concentration and dilution with acetoneitrile. A HPLC with UV detection at 220 nm and a Waters Sun FireTM-C18 column, which was eluted with methanol and 0.5% phosphoric acid aqueous solution and was used based on an external standard calibration curve. [Results] The results showed that the average recoveries were 88.4-95.6% for beet plants and 91.2-91.8% for soils. The relative standard deviations were 2.0-4.5% and 4.3-5.3% respectively. The minimum detectable level was 1.6×10-10g, the lowest detectable concentration was 0.02mg/kg. [Conclusions] The method is convenient and can meet the requirement of residual analysis and also provide reference for other crops.


2015 ◽  
Vol 51 (4) ◽  
pp. 823-832 ◽  
Author(s):  
Francine Rodrigues Ianiski ◽  
Luciane Varini Laporta ◽  
Alexandre Machado Rubim ◽  
Cristiane Luchese

abstract A method to ensure that an analytical method will produce reliable and interpretable information about the sample must first be validated, making sure that the results can be trusted and traced. In this study, we propose to validate an analytical high performance liquid chromatography (HPLC) method for the quantitation of meloxicam loaded PEGylated nanocapsules(M-PEGNC). We performed a validation study, evaluated parameters including specificity, linearity, quantification limit, detection limit, accuracy, precision and robustness. PEGylated nanocapsules were prepared by interfacial deposition of preformed polymer, and the particle size, polydispersity index, zeta potential, pH value and encapsulation efficiency were characterized. The proposed HPLC method provides selective, linear results in the range of 1.0-40.0 μg/mL; quantification and detection limits were 1.78 μg/mL and 0.59 μg/mL, respectively; relative standard deviation for repeatability was 1.35% and intermediate precision was 0.41% and 0.61% for analyst 1 and analyst 2, respectively; accuracy between 99.23 and 101.79%; robustness between 97.13 and 98.45% for the quantification of M-PEGNC. Mean particle diameters were 261 ± 13 nm and 249 ± 20 nm, polydispersity index was 0.15 ± 0.07 and 0.17 ± 0.06, pH values were 5.0 ± 0.2 and 5.2 ± 0.1, and zeta-potential values were -37.9 ± 3.2 mV e -31.8 ± 2.8 mV for M-PEGNC and placebo(B-PEGNC), respectively. In conclusion, the proposed analytical method is suitable for the quality control of M-PEGNC. Moreover, suspensions showed monomodal size distributions and low polydispersity index indicating high homogeneity of formulations with narrow size distributions, and appropriate pH and zeta potential. The extraction process was efficient for release of meloxicam from nanostructured systems.


2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%~105.7%,the relative standard deviation(RSD)wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.


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