scholarly journals Determination of Cassiarin A Level of Cassia siamea Leaf Obtained from Various Regions in Indonesia Using the TLC-Densitometry Method

2020 ◽  
Vol 2020 ◽  
pp. 1-7
Author(s):  
Wiwied Ekasari ◽  
Yuli Widiyastuti ◽  
Dyah Subositi ◽  
Rini Hamsidi ◽  
Aty Widyawaruyanti ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Antimalarial Activity ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Limit Of Quantification ◽  
Cassia Siamea ◽  
Limit Of Quantitation

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.

scholarly journals Development and Validation of HPTLC Method for Estimation of Carbamazepine in Formulations and Its In Vitro Release Study

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Rashmin B. Patel ◽  
Mrunali R. Patel ◽  
Kashyap K. Bhatt ◽  
Bharat G. Patel
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
In Vitro Release ◽  
Analysis Data ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Development And Validation ◽  
Vitro Release

A new, simple, and rapid high-performance thin-layer chromatographic method was developed and validated for quantitative determination of Carbamazepine. Carbamazepine was chromatographed on silica gel 60 F254 TLC plate using ethyl acetate-toluene-methanol (5.0 + 4.0 + 1.0 v/v/v) as mobile phase. Carbamazepine was quantified by densitometric analysis at 285 nm. The method was found to give compact spots for the drug (Rf=0.47 ± 0.01). The linear regression analysis data for the calibration plots showed good linear relationship with r2=.9995 in the concentration range 100–600 ng/spot. The method was validated for precision, recovery, repeatability, and robustness as per the International Conference on Harmonization guidelines. The minimum detectable amount was found to be 16.7 ng/spot, whereas the limit of quantitation was found to be 50.44 ng/spot. Statistical analysis of the data showed that the method is precise, accurate, reproducible, and selective for the analysis of Carbamazepine. The method was successfully employed for the estimation of equilibrium solubility, quantification of Carbamazepine as a bulk drug, in commercially available preparation, and in-house developed mucoadhesive microemulsion formulations and solution.

scholarly journals Application of a Stability-Indicating Thin-Layer Chromatographic Method to the Determination of Tenatoprazole in Pharmaceutical Dosage Forms

2009 ◽  
Vol 92 (2) ◽  
pp. 387-393 ◽  
Author(s):  
Sunil R Dhaneshwar ◽  
Vidhya K Bhusari ◽  
Mahadeo V Mahadik ◽  
B Santakumari
Keyword(s):  
Thin Layer ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Pharmaceutical Dosage Forms ◽  
Mean Values ◽  
Stability Indicating ◽  
Limit Of Quantitation

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.

scholarly journals UPLC Method Development and Validation for the Determination of Chlophedianol Hydrochloride in Syrup Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 25-31
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Calibration Plot ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

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.

scholarly journals DEVELOPMENT AND VALIDATION OF ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF FEBUXOSTAT FOR CONDUCTING IN-VITRO QUALITY CONTROL TESTS IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 115
Author(s):  
Jaspreet Kaur ◽  
Daljit Kaur ◽  
Sukhmeet Singh
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation

Objective: A simple, accurate, and selective ultraviolet-spectrophotometric method has been developed for the estimation of febuxostat in the bulk and pharmaceutical dosage forms.Method: The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines. The developed method was validated statistically with respect to linearity, range, precision, accuracy, ruggedness, limit of detection (LOD), limit of quantitation (LOQ), and recovery. Specificity of the method was demonstrated by applying different stressed conditions to drug samples such as acid hydrolysis, alkaline hydrolysis, oxidative, photolytic, and thermal degradation.Results: The study was conducted using phosphate buffer pH 6.8 and λmax was found to be 312 nm. Standard plot having a concentration range of 1–10 μg/ml showed a good linear relationship with R2=0.999. The LOD and LOQ were found to be 0.118 μg/ml and 0.595 μg/ml, respectively. Recovery and percentage relative standard deviations were found to be 100.157±0.332% and <2%, respectively.Conclusion: Proposed method was successfully applicable to the pharmaceutical formulations containing febuxostat. Thus, the developed method is found to be simple, sensitive, accurate, precise, reproducible, and economical for the determination of febuxostat in pharmaceutical dosage forms.

Quantification of Newly Discovered Anti-Cancer Drug Enzalutamide in Bulk and Synthetic Mixture by Stability Indicating TLC Method

2019 ◽  
Vol 16 (1) ◽  
pp. 104-112
Author(s):  
Dharmendra Jayantibhai Prajapati ◽  
Usmangani Khalilurraheman Chhalotiya ◽  
Minesh Dahyabhai Prajapati ◽  
Jalpa Upendrabhai Patel ◽  
Jaineel Vinodrai Desai
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Solvent System ◽  
Chemical Oxidation ◽  
Synthetic Mixture ◽  
Cancer Drug ◽  
Limit Of Quantification ◽  
Stability Indicating

Objective: An impressionable, discriminatory and precise stability indicating high performance thin layer chromatographic method has been developed and validated for the estimation of Enzalutamide in bulk and synthetic mixture. Method: The method engaged HPTLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase while the solvent system was ethyl acetate: toluene (4.5:5.5, v/v). The Rf value of enzalutamide was detected to be 0. 39 &amp;#177; 0. 005 and the densitometric analysis was carried out in absorbance mode at 246 nm. The linear regression analysis data for the calibration plots presented a virtuous linear relationship for enzalutamide over a concentration range of 20 - 1000ng/band. Results: The limit of detection and limit of quantification for enzalutamide was found to be 9.05 and 27.43 ng/band. Enzalutamide was imperilled to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photolytic degradation. The degraded product peaks were well resolved from the pure drug peak with substantial difference in their Rf values. Conclusion: Stressed samples were assayed using developed TLC technique. Suggested method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of enzalutamide in synthetic mixture.<P&gt;

scholarly journals Determination of Diazepam in Cream Biscuits by Liquid Chromatography

2004 ◽  
Vol 87 (3) ◽  
pp. 569-572 ◽  
Author(s):  
Priyankar Ghosh ◽  
Mudiam Mohanakrishna Reddy ◽  
Beedu Sashidhar Rao ◽  
Rajendra Kumar Sarin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Internal Standard ◽  
Reversed Phase ◽  
Calibration Plot ◽  
Relative Standard ◽  
Limit Of Quantitation

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.

scholarly journals Isolation and TLC Densitometric Quantification of Lysergol from the Seeds of Ipomoea muricata (Linn.) Jacq.

2013 ◽  
Vol 2013 ◽  
pp. 1-6
Author(s):  
Shrikant Patil ◽  
Manish Nivsarkar ◽  
Sheetal Anandajiwala
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Indole Alkaloids ◽  
Analysis Data ◽  
Phase Plate ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Chloroform Methanol ◽  
Instrumental Precision

Seeds of Ipomoea muricata, well known in Ayurveda for its purgative action, contains mainly indole alkaloids. Lysergol (major alkaloid) exhibits hypotensive, psychotropic, and uterus and intestine-stimulating properties. TLC fingerprint profile of I. muricata seeds was developed using chloroform : methanol (95 : 5 v/v) as the mobile phase. Plate was visualized under UV 254 nm and UV 366 nm and after derivatization with Van Urk reagent. Lysergol resolved at . Further, TLC-densitometric method was developed and validated for quantification of Lysergol avoiding derivatization step. Ethyl acetate :  methanol (7 : 3 v/v) was used as the mobile phase. Linear regression analysis data for the calibration curve showed a good linear relationship () in the concentration range from 20 ng to 140 ng, with respect to the peak area. The developed method was precise with RSD for intraday (range from 1.20 to 1.89) and interday (range from 1.39 to 1.92) for 60, 80, and 100 ng/spot of Lysergol. The instrumental precision was 0.67 (% RSD). The limit of detection and limit of quantification for Lysergol were 12 ng and 40 ng, respectively. The average percentage recovery was 99.68. The amount of Lysergol was found to be 0.23% w/w. To the best of our knowledge, this is the first report for the quantification of Lysergol from I. muricata seeds without derivatization.

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
Keyword(s):  
Formic Acid ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Calibration Plot ◽  
Tlc Plates ◽  
Acacia Catechu ◽  
Hptlc Method

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.

scholarly journals In Vitro and In Vivo Correlation of Colon-Targeted Compression-Coated Tablets

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Siddhartha Maity ◽  
Amit Kundu ◽  
Sanmoy Karmakar ◽  
Biswanath Sa
Keyword(s):  
Drug Release ◽  
Drug Absorption ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Absorption Study ◽  
Limit Of Quantification ◽  
In Vitro Drug Release

This study was performed to assess and correlate in vitro drug release with in vivo absorption of prednisolone (PDL) from a colon-targeted tablet prepared by compression coating of core tablet. In vivo drug absorption study was conducted using a high performance liquid chromatographic (HPLC) method, which was developed and validated for the estimation of PDL in rabbit plasma. The calibration curve showed linearity in the concentration range of 0.05 to 50 μg/mL with the correlation coefficient (r) of 0.999. The method was specific and sensitive with the limit of detection (LOD) and lower limit of quantification (LLOQ) of 31.89±1.10 ng/mL and 96.63±3.32 ng/mL, respectively. The extraction recovery (ER) of PDL from three different levels of quality control (QC) samples ranged from 98.18% to 103.54%. In vitro drug release study revealed that less than 10% drug was released in 6.34 h and almost complete (98.64%) drug release was achieved in the following 6 h. In vivo drug absorption study demonstrated lower values of Cmax, AUCtotal, and protracted Tmax from compression-coated tablet. The results confirmed the maximum release of drug in the colon while minimizing release in the upper gastrointestinal tract (GIT). An excellent in vitro and in vivo correlation (IVIVC) was also achieved after considering the lag time.

scholarly journals Challenges of HPLC Method Development and Validation for the Assay of Bemotrizinol from Complex Matrix in Cosmeceutical Preparation

2020 ◽  
Vol 11 (03) ◽  
pp. 310-316
Author(s):  
Kallol S Jana ◽  
Beduin Mahanti
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard

A simple high performance liquid chromatography (HPLC) method was developed for the assay of bemotrizinol (Tinosorb-S) from the complex pharmaceutical cosmetics matrix. Unlike the existing methods, the proposed mobile phase used in this method is very simple and excluding buffer. The use of buffer reducing column longevity and also a time-consuming process which increases the cost of analysis. To overcome all the referred problems, the present article was developed and validated as per International Council for Harmonization (ICH) guidelines. The reverse-phase chromatography was performed on Shimadzu model no. SPD-M10A VP with LC solution software, μBondapack (3.9 × 300 mm, 10-micron particle size) column with methanol (100%) as mobile phase at a flow rate 2.5 mL per minutes and UV detection at 254 nm. The retention time of bemotrizinol was found in 17.599 minutes, and the linear regression analysis data for the calibration plots showed a good linear relationship in the concentration range 70 to 130 μg/mL. The value of the correlation coefficient, slope, and intercept were 0.996, 7,715, and 15,320, respectively. The limit of quantification (LoQ) and limit of detection (LoD) were found to be 1.32 and 0.44, respectively. The relative standard deviation (RSD) for intra-day sample A 1.0858, sample B 0.8859, and inter-day sample A 0.9921, sample B 0.967 which were found to be lesser than 2%. The developed method was validated with regard to linearity, accuracy, precision, selectivity, and robustness, and the method was found to be simple, cost-effective, precise, accurate, linear, and specific for the successful identification and determination of bemotrizinol in pharmaceutical cosmetic preparation.

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