scholarly journals Estimation of Catechin in Ayurvedic Oil Formulations Containing Acacia catechu

2009 ◽  
Vol 92 (4) ◽  
pp. 1021-1026 ◽  
Author(s):  
Nidhi Dubey ◽  
Nitin Dubey ◽  
Rajendra Mehta ◽  
Ajay Saluja

Abstract A sensitive, simple, rapid, and efficient HPTLC method was developed and validated for the analysis of catechin in marketed Ayurvedic oil formulations containing Acacia catechu. Chromatography of methanolic0.1 formic acid (7:3, v/v) extracts of these formulations was performed on silica gel 60 F254 aluminum-backed TLC plates of 0.2 mm layer thickness. The plate was developed up to 85 mm with the ternarymobile phase chloroformacetone0.1 formic acid (7.7 + 1.5 + 0.8, v/v/v) at 22 2C with 20 min of chamber saturation. The system produced compact spots of catechin at an Rf value of 0.36. The marker, catechin, was quantified at its maximum absorbance of 296 nm. The limit of detection and quantitation values were 6 and 20 ng/spot, respectively. The linear regression analysis data for the calibration plot showed a good linear relationship with a correlation coefficient of 0.9993 in the concentration range of 2001200 ng/spot for catechin with respect to peak area. Repeatability of the method was 0.88 RSD. Recovery values from 97 to 102 indicate excellent accuracy of the method. The developed HPTLC method is accurate, precise, and cost-effective, and it can be successfully applied for the determination of catechin in marketed Ayurvedic oil formulations containing Acacia catechu.

2008 ◽  
Vol 91 (5) ◽  
pp. 1149-1153 ◽  
Author(s):  
Kedar Kumar Rout ◽  
Subhalaxmi Pradhan ◽  
Sagar Kumar Mishra

Abstract A sensitive, simple, rapid, and efficient high-performance thin-layer chromatographic (HPTLC) method has been developed and validated for the analysis of berberine in marketed Ayurvedic formulations containing Berberis aristata DC for regulatory purposes. Chromatography of methanolic extracts of these formulations was performed on silica gel 60 F254 aluminum-backed TLC plates of 0.2 mm layer thickness. The plate was developed up to 66 mm with the ternary-mobile phase butanolacetic acidwater (8 + 1 + 1, v/v/v) at 33 5C with 5 min of tank saturation. The marker, berberine, was quantified at its maximum absorbance of 350 nm. The limit of detection and limit of quantitation values were found to be 5 and 10 ng/spot. The linear regression analysis data for the calibration plot showed a good linear relationship with correlation coefficient 0.9994 in the concentration range of 10 to 50 ng/spot for berberine with respect to peak area. The instrumental precision was found to be 0.49 coefficient of variation (CV), and repeatability of the method was 0.73 CV. Recovery values from 98.27 to 99.11 indicate excellent accuracy of the method. The developed HPTLC method is very accurate, precise, and cost-effective, and it has been successfully applied to the assay of marketed formulations containing B. aristata for determination of berberine.


Author(s):  
Sunil Kaushik ◽  
Mohammad Asif

Solanesol is the starting material for many high value biochemicals, including Co-enzyme Q10 and vitamin-K analogues. The aim of the current study was to develop and validate a reliable and fast analytical procedure for the determination of solanesol in Nicotianatabacum using high-performance thin layer chromatography (HPTLC) method. The method was developed on TLC aluminium plates precoated with silica gel 60F-254 using solvent system hexane: ethyl acetate (5:1, v/v), which gives compact spot of solanesol (Rf value 0.41 ± 0.02). Densitometric analysis of solanesol was carried out in the absorbance mode at 210 nm. The linear regression analysis data for the calibration plot showed good linear relationship with r = 0.9978 with respect to peak area, in the concentration rang 100-5000 ng per spot of solanesol. The limit of detection and quantification were 13 and 30 ng per spot, respectively. The proposed method was applied for quantitative estimation of solanesol in different parts of Nicotianatabacum from different geographical regions in India, which showed that maximum amount of solanesol was found to be present in leaf sample collected from Karnataka i.e. 3.52 mg/g. Statistical analysis proved that the method is repeatable, selective and accurate for the estimation of solanesol in Nicotianatabacum.


Author(s):  
Anas Rasheed ◽  
Osman Ahmed

A specific, precise, accurate ultra pressure liquid chromatography (UPLC) method is developed for estimation of chlophedianol hydrochloride in bulk drug and syrup dosage form. The method employed with Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) in a gradient mode, with mobile phase of methanol and acetonitrile in the ratio of 65:35 %v/v. The flow rate was 0.1 ml/min and effluent was monitored at 254 nm. Retention time was found to be 1.130±0.005 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ)in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was good linear relationship between response and concentration in the range of 20-100 μg/ml respectively. The LOD and LOQ values were found to be 2.094(μg/ml)and 6.3466(μg/ml)respectively. No chromatographic interference from syrup excipients and degradants were found. The proposed method was successfully used for estimation of chlophedianol hydrochloride in syrup dosage form.


2018 ◽  
Vol 9 (2) ◽  
pp. 115-120 ◽  
Author(s):  
Mohammed Al Bratty ◽  
Safaa Fathy Saleh ◽  
Hassan Ahmad Alhazmi ◽  
Sadique Akhtar Javed ◽  
Adel Mohammed Ahmed ◽  
...  

The main purpose of the present study was to develop and validate a high performance thin layer chromatographic (HPTLC) method for quantitative determination of an antiviral agent, zanamivir in pure drug and diskhaler powder formulation. Chromatography was performed on aluminum TLC plates pre-coated with silica gel 60F254, employing a mixture of chloroform:methanol:ammonia (9.5:3.2:0.2,v:v:v) as mobile phase. The TLC scanner was operated in the absorbance mode at a wavelength of 230 nm for evaluation of chromatograms. The system has given well resolved peak of zanamivir (Rf = 0.56). The linearity of the method was established in the range of 20-300 ng/spot; correlation coefficient (r) was 0.9995. The low values of limit of detection and limit of quantification (12.4 and 37.5 ng/spot, respectively) have demonstrated the sensitivity of the developed method. The reported method was precise in both intra-day as well as inter-day analysis; % RSD of peak area was found to be less than 2%, and has an accuracy within 100 ± 2%. The developed method has a potential to quantify zanamivir from its diskhaler formulation without any interference from other components. The applicability of the method was demonstrated by excellent recovery of analyte (99.8%) from diskhaler formulation. The current analytical method can be applied for routine analysis of zanamivir in pure form and pharmaceutical formulation in quality control laboratories. 


2009 ◽  
Vol 92 (2) ◽  
pp. 387-393 ◽  
Author(s):  
Sunil R Dhaneshwar ◽  
Vidhya K Bhusari ◽  
Mahadeo V Mahadik ◽  
B Santakumari

Abstract A sensitive, selective, precise, and stability-indicating thin-layer chromatographic (TLC) method was developed and validated for the determination of tenatoprazole both as a bulk drug and in formulation. The method uses TLC aluminum plates precoated with Silica Gel 60F-254 as the stationary phase and the solvent system tolueneethyl acetatemethanol (6 4 1, v/v/v). This system gave compact spots for tenatoprazole (Rf value of 0.34 0.02). Tenatoprazole was subjected to acid and alkali hydrolysis, oxidation, and photodegradation. The peaks of the degradation products were well-resolved from that of the pure drug and had significantly different Rf values. Densitometric analysis of tenatoprazole was performed in the absorbance mode at 306 nm. The linear regression analysis data for the calibration plots showed a good linear relationship over the concentration range of 1001500 ng/spot. The mean values of the correlation coefficient, slope, and intercept were 0.9989 1.42, 10.27 0.965, and 4894.2 1.24, respectively. The method was validated for precision, robustness, and recovery. The limit of detection and limit of quantitation were 50 and 100 ng/spot, respectively. Statistical analysis showed that the method is repeatable and selective for estimation of tenatoprazole. Because the method can separate the drug from its degradation products, it can be used to monitor stability.


2004 ◽  
Vol 87 (3) ◽  
pp. 569-572 ◽  
Author(s):  
Priyankar Ghosh ◽  
Mudiam Mohanakrishna Reddy ◽  
Beedu Sashidhar Rao ◽  
Rajendra Kumar Sarin

Abstract An analytical procedure was developed for the detection and quantitation of diazepam in cream biscuits, which were used to commit crime. The method involves the extraction of diazepam with ethanol at room temperature, and the extract is filtered, evaporated to dryness, and redissolved in the mobile phase, methanol–acetonitrile–tetrahydrofuran–water (15 + 55 + 4 + 26, v/v). The separation is achieved on a C18 reversed-phase column with the mobile phase and diode array detection (λmax) at 230 nm. Medazepam is used as the internal standard is for quantification. The calibration plot for the determination of diazepam is based on linear regression analysis (y = 0.6687x + 0.0372; r2 = 0.995). The limit of detection for diazepam in the biscuit samples was estimated as 600 ng/mL. The limit of quantitation for diazepam was estimated as 1.75 μg/mL. The diazepam detected per piece of biscuit was found to be in the range of 0.27–0.45 mg. Pure diazepam was added to biscuit samples at 3 levels (100 and 500 μg/g, and 1 mg/g), and the recoveries were found to be 95%. The mean retention time of diazepam was 2.7 min and that of medazepam (IS) was 4 min. The relative standard deviations of the diazepam level in the biscuit samples were estimated to be 0.4% for retention time and 1.02% for peak area in intraday analysis, whereas the corresponding values were and 0.61 and 2.34% in interday analysis. The method is rapid and reliable for qualitative and quantitative analysis of cream biscuits laced with diazepam, and it can be used by law enforcement laboratories for routine analysis.


2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Wiwied Ekasari ◽  
Yuli Widiyastuti ◽  
Dyah Subositi ◽  
Rini Hamsidi ◽  
Aty Widyawaruyanti ◽  
...  

Cassia siamea leaf has been proven in vitro and in vivo to have a strong antimalarial activity with Cassiarin A as its active compound. To obtain a source of C. siamea medicinal plant with high level of active antimalarial compound (Cassiarin A), a valid method for determining Cassiarin A level is needed. For this reason, this research conducts the validation of the Cassiarin A content with determination method using thin-layer chromatography (TLC) densitometry which includes the determination of selectivity (Rs), linearity (r), accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). Cassiarin A was chromatographed on silica gel 60 F254 TLC plate using chloroform : ethanol (85 : 15 v/v) as a mobile phase. Cassiarin A was quantified by densitometric analysis at 368 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r = 0.9995. The method was validated for precision, recovery, repeatability. The minimum detectable amount was found to be 0.0027 μg/spot, whereas the limit of quantitation was found to be 0.008 μg/spot. The results of this validation are then used to determine the Cassiarin A level of C. siamea leaf from various regions in Indonesia. Based on the results of the study, it can be concluded that the TLC-densitometry method can be used to determine level of the Cassiarin A compound with the advantages of being fast, easy, accurate, and inexpensive. In addition, it showed that C. siamea leaves from Pacitan have the highest level of Cassiarin A compared to other areas studied.


2017 ◽  
Vol 100 (5) ◽  
pp. 1400-1406 ◽  
Author(s):  
Khalid A M Attia ◽  
Nasr M El-Abasawi ◽  
Ahmed El-Olemy ◽  
Ahmed H Abdelazim

Abstract HPLC method was developed for the selective determination of phenazopyridine hydrochloride (PAP) in the presence of its computationally selected metabolite. Density functional theory was applied as a computational model to study the energy of PAP metabolites, and the results revealed that 2,3,6-triaminopyridine (TAP) is the most stable metabolite. Good resolution and separation of PAP from TAP was achieved using a reversed-phase BDS Hypersil C18 column with a mobile phase consisting of acetonitrile–water (75 + 25, v/v) at flow rate of 1 mL/min and with UV detection at 280 nm. The linear regression analysis data for the calibration plot of PAP showed a good linear relationship over the concentrationrange of 5–45 μg/mL, with an LOD of 0.773 μg/mL. Moreover, a theoretical investigation of the relationship between the stationary phaseand the studied molecules was performed to confirm the experimental results. The proposed method was successfully applied for the selective determination ofPAP in pharmaceutical formulation. In addition, the obtained results were statistically compared to a reported method, with no significant differences foundbetween the investigated method and the reported onewith respect to accuracy and precision.


2019 ◽  
Vol 9 (6) ◽  
pp. 169-172
Author(s):  
Mohal Lal ◽  
Aboli Kadam ◽  
Aishwarya S. Padole

A new, simple, sensitive, selective, precise and robust high-performance thin-layer chromatographic (HPTLC) method for analysis of stigmasterol was developed and validated for the determination of stigmasterol in different extracts. A new, simple, sensitive, selective, precise and robust high-performance thin-layer chromatographic (HPTLC) method for analysis of stigmasterol was developed and validated for the determination of stigmasterol in different extracts. Analysis of stigmasterol was performed on TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. Linear ascending development was carried out in twin trough glass chamber saturated with mobile phase consisting of Hexane : Acetone (8:2 v/v) at room temperature. (25 °C ± 2 °C) Camag TLC scanner III was used for spectrodensitometric scanning and analysis in absorbance mode at 490nm. The system was found to give compact spots for stigmasterol. (Rf value of 0.44 ± 0.02) The linear regression analysis data for the calibration plots showed good linear relationship with r2 =0.9997 ± 0.0002 in the concentration range 200-1200 ng spot−1 with respect to peak area. According to the International Conference on Harmonization (ICH) guidelines the method was validated for precision, recovery and robustness. Statistical analysis of the data showed that the method is reproducible and selective for the estimation of stigmasterol. Keywords: Tagetes erecta, Capsicum annuum, stigmasterol, HPTLC, method validation


2010 ◽  
Vol 93 (3) ◽  
pp. 811-819 ◽  
Author(s):  
Rashmin B Patel ◽  
Mrunali R Patel ◽  
Kashyap K Bhatt ◽  
Bharat G Patel

Abstract A new, simple, and rapid HPTLC method was developed and validated for quantitative determination of olanzapine on silica gel 60F254 layers using methanolethyl acetate (8.0 + 2.0, v/v) as the mobile phase. Olanzapine was quantified by densitometric analysis at 285 nm. The method was found to give compact bands for the drug (Rf = 0.35 0.02). The linear regression analysis data for the calibration plots showed a good linear relationship with r2 = 0.9997 in the concentration range of 100600 ng/band. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The LOD was found to be 23.90 ng/band, and the LOQ was 91.04 ng/band. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of olanzapine. The method was successfully used for the determination of equilibrium solubility and quantification of olanzapine as a bulk drug, in a commercially available preparation, and in in-house developed mucoadhesive microemulsion formulations and solution.


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