scholarly journals Chromatographic methods for determination of finasteride and tamsulosin hydrochloride and in presence of finasteride degradation product

2020 ◽  
Vol 32 (2) ◽  
pp. 95-101 ◽  
Author(s):  
Hany H. Monir ◽  
Alshimaa M. Ali ◽  
Rawnaa E. Refat ◽  
Samah S. Abbas
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Uv Detection ◽  
Hplc Separation ◽  
Chromatographic Methods ◽  
Bulk Powder ◽  
Ich Guidelines ◽  
Aluminum Plates ◽  
Layer Chromatography

Two sensitive and selective chromatographic methods were developed for determination of finasteride and tamsulosin hydrochloride in bulk powder and a pharmaceutical formulation. The first method was based on high-performance liquid chromatography (HPLC) separation of the cited drugs in the presence of the acid degradation product of finasteride. The separation was achieved using a C18 column (300 mm × 3.9 mm; 10-μm particle size) and a mobile phase consisting of 0.04 M ortho-phosphoric acid (pH 3.5 ± 0.2 adjusted with triethylamine) and acetonitrile (50:50, v/v). Quantification was achieved with ultraviolet (UV) detection at 215 nm. Linearity was in the range of 10.00–110.00 μg/mL and 2.00–44.00 μg/mL for finasteride and tamsulosin hydrochloride, respectively. Thin-layer chromatography (TLC)–densitometric method was achieved on an aluminum plates pre-coated with silica gel 60 F254 using toluene–ethanol–diethylamine (8:2:1.5, by volume) as eluent, and the RF values of tamsulosin hydrochloride and finasteride were 0.57 and 0.64, respectively. Quantification was achieved with UV detection at 250 nm for finasteride and 280 nm for tamsulosin hydrochloride. Linearity was in the range of 1.00–40.00 and 0.2.00–20.00 μg per spot for finasteride and tamsulosin hydrochloride, respectively. The results obtained were validated according to the International Conference on Harmonisation (ICH) guidelines. A statistical comparison between the obtained results and the results of a reported method was carried out.

Two Validated Chromatographic Methods for Determination of Ciprofloxacin HCl, One of its Specified Impurities and Fluocinolone Acetonide in Newly Approved Otic Solution

2021 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Israa A Wahba ◽  
Samah S Saad ◽  
Nesrin K Ramadan
Keyword(s):  
High Performance ◽  
Fluocinolone Acetonide ◽  
Ultraviolet Detection ◽  
Chromatographic Methods ◽  
Bulk Powder ◽  
Developing System ◽  
Layer Chromatography ◽  
Chloroform Methanol ◽  
Linear Regressions

Abstract Two sensitive, selective and precise chromatographic methods have been established for concomitant quantification of ciprofloxacin HCl (CIP), fluocinolone acetonide (FLU) along with ciprofloxacin impurity A (CIP-imp A). The first method was thin-layer chromatography (TLC-densitometry) where separation was accomplished using TLC silica plates 60 G.F254 as a stationary phase and chloroform–methanol–33%ammonia (4.6:4.4:1, by volume) as a developing system. The obtained plates were scanned at 260 nm over concentration ranges of 1.0–40.0, 0.6–20.0 and 1.0–40.0 μg band−1 for CIP, FLU and CIP-imp A, respectively. The second method was based on high-performance liquid chromatography using a Zorbax ODS column (5 μm, 150 × 4.6 mm i.d.) where adequate separation was achieved through a mobile phase composed of phosphate buffer pH 3.6–acetonitrile (45:55, v/v) at flow rate 1.0 mL min−1 with ultraviolet detection at 254 nm. Linear regressions were obtained in the range of 1.0–40.0 μg mL−1 for CIP, 0.6–20.0 μg mL−1 for FLU and 1.0–40.0 μg mL−1 for CIP-imp A. The suggested methods were validated in compliance with the International Conference on Harmonization guidelines and were successfully applied for determination of CIP and FLU in bulk powder and newly marketed otic solution.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

scholarly journals IDENTIFICATION, QUANTIFICATION AND VALIDATION OF STIGMASTEROL FROM ALPINIA CALCARATA USING HIGH-PERFORMANCE THIN LAYER CHROMATOGRAPHY METHOD

2017 ◽  
Vol 9 (9) ◽  
pp. 126
Author(s):  
Pratheema Philomindoss
Keyword(s):  
Linear Regression ◽  
Thin Layer ◽  
Linear Relationship ◽  
High Performance ◽  
Retention Factor ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Layer Chromatography ◽  
Hptlc Method

Objective: The present study is designed to develop a new simple, precise, rapid and selective high‐performance thin‐layer chromatographic (HPTLC) method for the determination of stigmasterol in methanolic rhizomes extract of Alpinia calcarata.Methods: As per International Conference on Harmonization (ICH) guidelines we have applied different concentrations of stigmasterol as standard on HPTLC plates for the quantification of stigmasterol from the Alpinia calcarata rhizomes. The concentration of standard stigmasterol is 1 mg/ml.Results: The retention factor of stigmasterol was 0.58. Linearity was obtained in the range of 50 ng‐250 ng for stigmasterol. The developed and validated HPTLC method was employed for stigmasterol in methanolic rhizomes extract of Alpinia calcarata for standardization of the content of the marker. The linear regression data for the calibration plots showed a good linear relationship with r=0.99977 for stigmasterol, respectively Satisfactory recoveries of 99.77 % were obtained for stigmasterol.Conclusion: The results obtained in validation assays indicate the accuracy and reliability of the developed HPTLC method for the quantification of stigmasterol in methanolic rhizomes extract of Alpinia calcarata

scholarly journals Fingerprint Study of Curcuma xanthorrhiza Rhizome by High Performance Thin Layer Chromatography (HPTLC)

2016 ◽  
Vol 1 (2) ◽  
pp. 9-14
Author(s):  
Tina Wikara ◽  
Anny Sulistiowaty ◽  
Sri Murhandini ◽  
Tepy Usia
Keyword(s):  
High Performance ◽  
Phytochemical Analysis ◽  
Hptlc Plate ◽  
Spot Detection ◽  
Ich Guidelines ◽  
Curcuma Xanthorrhiza ◽  
Layer Chromatography ◽  
Chloroform Methanol

The rhizome of Curcuma xanthorrhiza Roxb is intensively used in Indonesia as traditional medicine. It is widely used for hepatoprotective and anti inflammatory activities. To ensure the quality of its extract, we have studied the fingerprint or phytochemical analysis. This research was aimed to produce a chromatogram profile of the rhizome by HPTLC. The HPTLC fingerprint chromatogram of C. xanthorrhiza rhizome was performed using HPTLC plate of silica gel 60 F254 as the stationary phase and chloroform-methanol (97:3) as the mobile phase. Spot detection was carried out by TLC photo documentary system at 254 and 366 nm and TLC scanner at 427 nm. The developed method was validated according to ICH guidelines by determination of specificity and precision. We found that the specifity and precission of the method were met the acceptance criteria. In conclusion, the developed method is valid and could be used for quality control and standardization of herbal medicine containing C. xanthorrhiza rhizome.

scholarly journals Chromatographic Methods for the Determination of Aminexil, Pyridoxine, and Niacinamide in a Novel Cosmetic Hair Preparation

2020 ◽  
Vol 103 (4) ◽  
pp. 1167-1172
Author(s):  
Mamdouh R Rezk ◽  
Hebatallah M Essam ◽  
Enas A Amer ◽  
Dina M S Youssif
Keyword(s):  
High Performance ◽  
High Sensitivity ◽  
Ammonia Solution ◽  
Hplc Method ◽  
The Novel ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Sensitivity And Selectivity ◽  
Keratin Fibers

Abstract Background Aminexil, a new compound patented by L’Oreal, has a stimulating effect on human keratin fibers. Pyridoxine HCl and niacinamide are added to boost the hair tonic effect of aminexil. Objective Two novel chromatographic methods were developed for the determination of aminexil (AX), niacinamide (NA) and pyridoxine HCl (PD) in the novel hair tonic preparation. Methods The developed methods were high-performance liquid chromatography (HPLC) and thin layer chromatography (TLC) with densitometric determination. Different experimental parameters were investigated and optimized to achieve complete baseline separation and well resolved peaks. The RP-HPLC separation was achieved using a Thermoscientific BDS hypersil C18 (250 × 4.6 mm, 5 µm) column using 0.005 M hexane sulfonic acid: methanol (80: 20, v/v) as a mobile phase. For the TLC method, the three analytes were partitioned between propanol: toluene: ammonia solution (40:60:2, v/v/v) and fluorescent silica plates. The two methods were validated in compliance with International Conference on Harmonization (ICH) guidelines. The obtained data were statistically analyzed to confirm the existing results. The developed methods were successfully applied for determination of the studied drugs in pure forms and in the cosmetic preparation. Results For the HPLC method, the RSDs of AX, NA and PD were 0.70, 0.88 and 1.17 respectively. For the TLC method, the RSDs of AX, NA and PD were 1.06, 1.37 and 0.73 respectively. Conclusions The proposed chromatographic methods showed high sensitivity and selectivity for the three compounds under analysis in the laboratory prepared mixture and in the hair tonic preparation. Highlights Aminexil, Pyridoxine, Niacinamide, HPLC. The present work offers two reproducible, accurate, validated, time and cost saving alternatives for the quantitative and qualitative determination of medicated hair preparation.

scholarly journals A Validated High Performance Thin Layer Chromatographic Method for Simultaneous Estimation of Berberine Chloride and Guggulsterone Z in Herbal Formulation

2019 ◽  
Vol 7 (1) ◽  
pp. 7-13
Author(s):  
Vijaykumar K. Parmar ◽  
Deepika Mohanta ◽  
Harsh Shah
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Simultaneous Estimation ◽  
Berberine Chloride ◽  
Herbal Formulation ◽  
Ich Guidelines ◽  
System Suitability ◽  
Layer Chromatography ◽  
Hptlc Method

A simple, precise, and robust high-performance thin layer chromatography (HPTLC) method was developed and validated for the determination of berberine chloride and guggulsterone Z in herbal formulation. Chromatographic separation was achieved on aluminium plates precoated with silica gel G60F254 as the stationary phase and toluene-acetonitrile-formic acid (5:3:0.5 v/v/v) as the mobile phase. Densitometric evaluation was carried out at 264 nm. The present method was validated according to ICH guidelines. The Rf value of berberine chloride and guggulsterone Z was found to be 0.40 ± 0.02 and 0.68 ± 0.02, respectively. The response in terms of peak area was found to be linear over the concentration range of 100-500 ng/spot for berberine chloride and 200-1000 ng/spot for guggulsterone Z with regression coefficient value greater than 0.995 for both the phytoconstituents. The method was validated by determining its accuracy, precision, robustness, specificity and system suitability. The method was found to be accurate, precise and robust to carry out the simultaneous estimation of berberine chloride and guggulsterone Z. The developed method was successfully applied for the simultaneous estimation of berberine chloride and guggulsterone Z in herbal formulation.

scholarly journals Validated Chromatographic methods for estimation of Solanine in Mahamrutyunjaya rasa

2020 ◽  
Vol 2 (01) ◽  
Author(s):  
Pallavi Rai ◽  
Rahul Kaushik ◽  
Sadhana J. Rajput
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Therapeutic Window ◽  
Chromatographic Methods ◽  
Linearity Range ◽  
Ich Guidelines ◽  
Ld50 Value ◽  
Layer Chromatography ◽  
Chloroform Methanol ◽  
Solanum Indicum

Introduction: Mahamrutyunjaya rasa is a herbomineral ayurvedic formulation used for various indications like fever, pain, cardiac arrhythmia, etc. It contains Solanum indicum as one of the ingredients having anti-inflammatory, diuretic, and diaphoretic properties. Solanine is one of the active biomarkers for Solanum indicum. The therapeutic window of Solanine is very narrow, with the LD50 value of 3-6 mg/kg body weight in humans. Objective: Estimation of such biomarkers is very significant to avoid any adverse events due to the administration of ayurvedic preparations containing Solanine. In the present study, two simple, sensitive, reliable chromatographic techniques have been developed and validated for the estimation of Solanine in Mahamrutyunjaya rasa. Materials and Methods: High-performance liquid chromatography (HPLC) separation of Solanine was performed on an reversed phase C-18 column (250 mm 9 4.6 mm ID, 5 lm particle size), with isocratic elution using a mixture of Tris buffer (10mM, pH 6.00): Acetonitrile(60:40, v/v) at a flow rate of 1 mL/min with UV detection at 218 nm for solanine. High-performance thin-layer chromatography (HPTLC) separation was done on Silica gel 60 F254 pre-coated plates using Chloroform: Methanol: Ammonia (7:3:0.5 v/v). The densitometric scanning was performed at 500 nm. The developed methods were validated for linearity, LOD, LOQ, accuracy, precision, and specificity as per ICH guidelines. Results: Solanine was eluted at 4.43 ± 0.1 min and established a linearity range of 1 – 100 μg/ml (r2 = 0.9992). In the HPTLC method, the Rf value of Solanine was 0.05 in a linearity range of 1600-4800 ng/ml. Conclusion: Reliable, rapid, simple, and sensitive chromatographic methods were developed for the quantification of Solanine in Mahamrutyunjaya Rasa.

scholarly journals Simultaneous Determination of Alprazolam and Fluoxetine Hydrochloride in Tablet Formulations by High-Performance Column Liquid Chromatography and High-Performance Thin-Layer Chromatography

2009 ◽  
Vol 92 (4) ◽  
pp. 1082-1088 ◽  
Author(s):  
Rashmin B Patel ◽  
Mrunali R Patel ◽  
Madhira B Shankar ◽  
Kashyap K Bhatt
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Uv Detection ◽  
Fluoxetine Hydrochloride ◽  
Phase Quantification ◽  
Tablet Formulations ◽  
Layer Chromatography

Abstract This paper describes validated HPLC and HPTLC methods for simultaneous determination of alprazolam (ALP) and fluoxetine hydrochloride (FXT) in pure powder and formulation. The HPLC separation was achieved on a Nucleosil C8 column (150 mm length, 4.6 mm id, 5 m particle size) using acetonitrilephosphate buffer pH 5.5 (45 + 55, v/v) as the mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The HPTLC separation was achieved on an aluminum-backed layer of silica gel 60F254 using acetonetolueneammonia (6.0 + 3.5 + 0.5, v/v/v) as the mobile phase. Quantification in the HPLC method was achieved with UV detection at 230 nm over the concentration range 414 g/mL for both drugs, with mean recovery of 99.95 0.38 and 99.85 0.56 for ALP and FXT, respectively. Quantification in the HPTLC method was achieved with UV detection at 230 nm over the concentration range of 4001400 ng/spot for both drugs, with mean recovery of 99.32 0.45 and 99.78 0.81 for ALP and FXT, respectively. These methods are simple, precise, and sensitive, and they are applicable for the simultaneous determination of ALP and FXT in pure powder and formulations.

scholarly journals Determination of Sucralose in Soft Drinks by High-Performance Thin-Layer Chromatography: Interlaboratory Study

2009 ◽  
Vol 92 (4) ◽  
pp. 1153-1159 ◽  
Author(s):  
Joerg Stroka ◽  
Ivanka Doncheva ◽  
Bernd Spangenberg ◽  
K Bouten ◽  
R Braemer ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
High Performance ◽  
Interlaboratory Comparison ◽  
Uv Detection ◽  
Regulatory Limits ◽  
European Regulatory ◽  
Cas Registry ◽  
Syringe Filter ◽  
Layer Chromatography

Abstract An interlaboratory comparison was carried out to evaluate the effectiveness of a method based on HPTLC in which reagent-free derivatization is followed by UV/fluorescence detection. The method was tested for the determination of sucralose (C12H19Cl3O8; (2R,3R,4R,5S,6R)-2- [(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan- 2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3, 4-diol; CAS Registry No. 56038-13-2) in carbonated and still beverages at the proposed European regulatory limits. For still beverages, a portion of the sample was diluted with methanolwater. For carbonated beverages, a portion of the sample was degassed in an ultrasonic bath before dilution. Turbid beverages were filtered after dilution through an HPLC syringe filter. The separation of sucralose was performed by direct application on amino-bonded (NH2) silica gel HPTLC plates (no cleanup needed) with the mobile phase acetonitrilewater. Sucralose was determined after reagent-free derivatization at 190C; it was quantified by measurements of both UV absorption and fluorescence. The samples, both spiked and containing sucralose, were sent to 14 laboratories in five different countries. Test portions of a sample found to contain no sucralose were spiked at levels of 30.5, 100.7, and 299 mg/L. Recoveries ranged from 104.3 to 124.6 and averaged 112 for determination by UV detection; recoveries ranged from 98.4 to 101.3 and averaged 99.9 for determination by fluorescence detection. On the basis of the results for spiked samples (blind duplicates at three levels), as well as sucralosecontaining samples (blind duplicates at three levels and one split level), the values for the RSDr ranged from 10.3 to 31.4 for determinations by UV detection and from 8.9 to 15.9 for determinations by fluorescence detection. The values for the RSDR values ranged from 13.5 to 31.4 for determinations by UV detection and from 8.9 to 20.7 for determinations by fluorescence detection.

scholarly journals Development and validation of high performance thin layer chromatographic method for the determination of voglibose in bulk and their formulations

2020 ◽  
Vol 9 (2) ◽  
pp. 1074-1078
Keyword(s):  
Thin Layer ◽  
High Performance ◽  
Chromatographic Method ◽  
Cost Effective ◽  
Band Size ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Aluminum Plates ◽  
Development And Validation

To develop a simple, fast, specific, precise and accurate High Performance Thin Layer Chromatographic method (HPTLC) for the determination of Voglibose in bulk and their dosage forms. The chromatographic separation was achieved on precoated silica gel 60F254 aluminum plates using a combination of acetonitrile: methanol: ammonia (15:4:0.1 % V/V/V) as mobile phase and densitometric evaluation of spots was carried out at 284 nm using Camag TLC scanner III with CATS 1.3.4 version software. The experimental parameters like band size of the chamber saturation time, spot application, slit width, solvent front migration, etc. were studied critically and evolved optimized conditions. The drug was well resolved satisfactorily with Rf value 0.66±0.03. The repeatability and accuracy of the optimized method were ascertained by evaluating various validation parameters like linearity (100 to 450 ng/spot), precision (intra-day % RSD 0.21 to 0.74, inter-day % RSD 0.21 to 0.29), accuracy (99.8% to 101.2%, % RSD below 1%), and specificity according to ICH guidelines. The limits of detection and quantification were 40 ng/spot and 100 ng/spot respectively. The developed HPTLC method was faster and cost effective quantitative control for routine analysis of Voglibose in bulk and its formulations.

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