Stability-indicating High Performance Thin Layer Research Articles

Principles of White Analytical Chemistry and Design of Experiments to Stability-Indicating Chromatographic Method for Simultaneous Estimation of Thiocolchicoside and Lornoxicam.

A variety of chromatographic methods have been published for the stability evaluation of thiocolchicoside and lornoxicam. Nevertheless, the development of chromatographic methods requires the use of neurotoxic and teratogenic organic solvents that are detrimental to the environment and harmful to human life. Using the principles of design of experiments (DoE), a novel white analytical chemistry-driven stability-indicating high-performance thin layer chromatographic (SI-HPTLC) method has been developed for the concurrent stability study of thiocolchicoside (THC) and lornoxicam (LNX). To protect the environment and human life, the stability-indicating HPTLC method was developed using safe organic solvents. Potential analytical method risk parameters (AMRPs) and analytical method performance attributes (AMPAs) were screened using the fractional factorial design. The response surface analysis and optimization of critical AMRPs and AMPAs was carried out using full factorial design. Navigation of the method operable design region (MODR) was used to develop the SI-HPTLC technique. The developed method was validated as per ICH (International council for harmonization) Q2(R1) guideline. The developed method's greenness was evaluated using AGREE (Analytical Procedure Greenness) tool and ESA (Eco-Scale Assessment). The Blue (B) model was used to assess the proposed method's cost and time efficiency and user-friendlyness. For the stability studies of THC and LNX, the twelve principles of WAC (White Analytical Chemistry) were used to evaluate the published and proposed chromatographic techniques. As compared to previously published chromatographic techniques for studying the stability of THC and LNX, the suggested approach was found to be more affordable, environmentally friendly, and user-friendly. Development of stability-indicating HPTLC method using a novel white analytical chemistry approach and organic solvents with low toxicity potential. Application of the developed method for analysis of the forced degraded sample and fixed-dose combinations of THC and LNX.

STABILITY INDICATING HPTLC METHOD FOR ESTIMATION OF BUDESONIDE AND FORMOTEROL FUMARATE DIHYDRATE IN PHARMACEUTICAL FORMULATION

A sensitive, selective, precise and accurate stability-indicating high-performance thin layer chromatographic method for analysis of budesonide (BUD) and formoterol fumarate dihydrate (FFD) was developed along with forced degradation study and validated according to ICH guidelines. Densitometry analysis of BUD and FFD was carried out in the absorbance mode at 234 nm using toluene: methanol: ethyl acetate: ammonia (8:2:2.5:0.1,% V/V/V/V) as solvent system. This system was found to give compact spots for BUD at Rf value of 0.34 ± 0.06 and FFD at Rf value of 0.67± 0.05. It was found that besides oxidative, thermal and photo stability studies, acid and base induced degradation of drugs were more with resultant degradation product. 32 factorial design was used to predict base induced degradation. The drug undergoes degradation under mainly acidic and basic conditions. Also, the degraded products were well resolved from the pure drugs with significantly different Rf values. Linearity was found to be in the range of 1800-10600 and 1000-6000 ng band-1 for BUD and FFD, respectively. The LOQ for BUD and FFD were 392.48 ng band-1 and 1189.36 ng band-1 and LOD for BUD and FFD was115.79 ng band-1 and 350.88 ng band-1, respectively. ‘‘Bartlett’s test’’ applied on peak area for linearity, additionally proved validity of the developed method. Good accuracy and precision were obtained as revealed from percentage RSD value less than 2. Similarly, no interference was observed from common excipients in tablet formulation as well as degradation product, indicating specificity of the method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one.

Development and Validation of a Stability-Indicating HPTLC Method for the Estimation of Eszopiclone in Pharmaceutical Dosage Forms

Objective: A simple, sensitive, selective, precise repeatable and stability-indicating high-performance thin layer chromatographic method was developed and validated for Eszopiclone in bulk drug and in formulation. Method: Silica gel 60 F-254, TLC precoated aluminium plates was used as the stationary phase for analyzing Eszopiclone and its degradation products, using mobile phase consisting toluene: ethyl acetate: methanol (6: 4: 2 v/v/v). Result: This mobile phase gave compact spots for Eszopiclone with Rf value of 0.52 ± 0.02. Eszopiclone was exposed to hydrolysis, oxidation, neutral and photolytic conditions for conducting stress degradation study. The peak of Eszopiclone and the degradation product was well resolved from each other with a significantly different Rf value. Densitometric estimation of Eszopiclone was performed at 304nm. A good linear plot was obtained in the concentration range of 150-300ng/spot. The method was validated for precision, accuracy (recovery) and robustness study. The limit of detection (LOD) and limit of quantitation (LOQ) was found to be 130ng/spot and 150ng/spot, respectively. Conclusion: The developed HPTLC method can separate Eszopiclone from its degradation products, hence stability studies can be performed using this method.

Development of Validated Stability-indicating High Performance Thin Layer Chromatography Method for Estimation of Rabeprazole Sodium and Aceclofenac in Bulk Drug

Objective: To develop a validated stability-indicating high performance thin layer chromatography method for the estimation of Rabeprazole Sodium (RZL) and Aceclofenac (ACF) in bulk drugs.
 Methods: A high performance thin layer chromatographic (HPTLC) method has been developed for the separation of RZL & ACF on plates precoated with aluminium back silica gel 60 F254. Different mobile phases were used on trial and error basis for separation of two drugs. The final mobile phase selected for analysis was toluene: ethyl acetate: methanol: acetic acid: ammonia in the ration of 6:4:1:0.2:0.1 (v/v). Both the drugs showed maximum absorbance at 279 nm which was selected as the detection wavelength throughout the experimental work. Developed method was validated as per ICH guidelines. Forced degradation of drugs was carried out under various stress conditions and HPTLC method was used for analysing the stability of drugs.
 Results: HPTLC method was successfully developed for separation of RZL and ACF with clear separation of bands of the drugs. Method validation after assessment of various parameters indicated low % RSD within an acceptable limit of < 2.0 and the stability studies indicated the satisfactory separation of both the drugs from that of degraded products with considerable % recovery profile.
 Conclusion: The developed method is rapid, reliable, precise, and reproducible and demonstrates the suitability of the method for stability determination of rabeprazole and aceclofenac.

Validated stability-indicating thin layer chromatographic determination of nadifloxacin in microemulsion and bulk drug formulations

A stability-indicating high performance thin layer chromatographic (HPTLC) method for the densitometric analysis of nadifloxacin in microemulsions was developed and validated according to the guidelines of the International Conference on Harmonization (ICH). The compact spot for nadifloxacin was found at an Rf value of 0.39±0.02 at an absorption wavelength of 288 nm using a mobile phase consisting of chloroform : methanol : formic acid (7.5 : 2.0 : 0.5 v/v). The linear regression data for the calibration plots (r 2= 0.9981) was found with respect to peak area in the concentration range of 50-600 ng/spot. The limit of detection (LOD) and limit of quantification (LOQ) were 9.4 and 20.5 ng respectively. The drug was subjected to acid and alkaline hydrolysis, oxidation, photo degradation and dry heat treatment. The peaks of degradation products were well-resolved from the peak of the standard drug with significantly different Rf values. Statistical analysis revealed that the developed HPTLC method is reproducible, selective and accurate for the determination of nadifloxacin in its formulations. The method can effectively separate the drug from its degradation products and be used for stability-indicating assay.

Novel Stability-Indicating High-Performance Thin Layer Chromatography (HPTLC) Method Development and Validation for Estimation of Daclatasvir Dihydrochloride in Pharmaceutical Dosage Form

Daclatasvir dihydrochloride (DTDH) is a direct-acting antiviral agent used against the hepatitis C Virus. Different analytical methods were reported for the determination of DTDH in pharmaceutical dosage form, including spectrophotometry, high-performance liquid chromatography (HPLC), and stability- indicating HPLC method but to date, no HPTLC method has been reported. A novel, simple, sensitive, selective, precise, and accurate stability-indicating high-performance thin-layer chromatographic (HPTLC) method has been developed for the quantification of Daclatasvir dihydrochloride (DTDH) in pharmaceutical formulation. Chromatography separation was carried out on pre-coated silica gel G60 F254 HPTLC plates using chloroform: methanol (9:1, v/v) as the mobile phase. Scanning and densitometric analysis were done at 316 nm. The band of DTDH were obtain at RF= 0.48±0.02. The calibration curve was plotted in the concentration range of 400– 900 ng/band and the method was found linear with r = 0.995. The LOD and LOQ were found to be 95 ng/band and 313.5 ng/band respectively. The percentage recovery was found to be 97.31-101.81 %. The developed was able to separate peaks of all the degradation products formed in ICH-prescribed stress conditions with a significant difference in their RF values. The developed method was validated according to ICH guidelines and results were found to be within acceptance criteria. The developed stability-indicating method successfully evaluated the DTDH in pharmaceutical tablet dosage form and assay results showed good recovery when statistically compared with the reversed-phase high-performance liquid chromatography (RP-HPLC) method.

Separation, Identification and Characterisation of Acidic Degradation of Ritonavir Under ICH Recommended Stress Condition by HPTLC, MS/TOF

The current study reports the characterization of degradation product from Ritonavir (RITO) through mass spectrometry and the development of a validated and stability-indicating High performance thin layer chromatographic method for the determination of RITO in the presence of its process-related degradation in bulk drug. Stability study on Ritonavir (RITO) was carried out under hydrolytic condition in acidic, alkaline and peroxide, thermal and photolytic conditions in accordance with International Conference on Harmonization (ICH) guidelines Q1 (R2). The drug was found susceptible for degradation under acidic conditions while in rest of conditions drug were stable. A degradation product (DP) was formed in acidic condition. Chromatographic separation was performed on precoated silica gel 60F254 HPTLC plates using acetonitrile: methanol: water (5:3.5:2.5 v/v) as a mobile phase. A mixture of stressed samples was subjected for IR and MS/TOF studies to obtain functional group and mass spectral data. The data found from precise mass study was first utilized to pattern a complete mass fragmentation pathway of the drug and later it was used for its degradant. Structures were proposed for each fragments based on best possible molecular formula. Acidic degradation of RITO 3((3S, 4R)-3-isopropyl-4-(((S)-2-((methoxycarbonyl) amino)-3-phenylpropyl) amino)-2-oxo-5-phenylpentyl)-1-((2isopropylthiazol-4-yl) methyl)-1-methyluronium was identified.

Development and Validation of a Stability-Indicating High Performance Thin Layer Chromatography (HPTLC) Method for estimation of Canagliflozin in bulk and Pharmaceutical Dosage Form

Cost-effectiveness analysis of Dapagliflozin versus Canagliflozin in treatment of type 2 diabetes mellitusSadagoban Gopal Krishnamoorthy, Jemi Rachel Shaji, Bhagya Premnath, Akshitha Rani Siby, Swathi Swaroopa Borra , Ayilya Manomohan, Arun Kanniyappan Parthasarathy

Development and Validation of Stability Indicating HPTLC Method for Estimation of Rizatriptan Benzoate in Bulk and Tablet Dosage Form

A new simple, accurate, precise and selective stability-indicating high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of Rizatiptan Benzoate in bulk and tablet formulation. Chromatographic separation was performed on aluminum plate precoated with Silica Gel 60 F254 using, Methanol: n-Propane: Triethylamine (3:5:2 v/v/v) as mobile phase followed by densitometric scanning at 280 nm. This system was found to give compact spot for Rizatiptan Benzoate (Rf value of Rf = 0.38 ± 0.02). The calibration curve was found to be linear between 800-2800 ng/band. The limit of detection and quantitation were found to be 2.24 ng/band and 6.79 ng/band respectively. The proposed method can be applicable for the estimation of Rizatiptan Benzoate during stability studies. Keywords: Rizatiptan Benzoate, High Performance Thin Layer Chromatography (HPTLC), Stability-Indicating Method

Application of a Validated Stability-Indicating HPTLC Method for Simultaneous Estimation of Paracetamol and Aceclofenac and their Impurities

A sensitive, accurate, precise and stability indicating HPTLC method has been developed and validated for the simultaneous determination of Paracetamol (PCT), Aceclofenac (ACF) and their impurities namely, 4-amino phenol (AP) and Diclofenac acid (DA), respectively, which are the hydrolytic degradation products and related substances of the drugs. The chromatographic separation was achieved using optimized mobile phase, ethyl acetate: methanol: glacial acetic acid (8.5:1.5:0.25 V/V) on pre-activated silica gel 60 F254 TLC plates with ultraviolet detection at 231 nm. Statistical analysis revealed linear relationships in the concentration ranges of 3900–9100, 1200–2800 for PCT, ACF respectively and 100-600 ng/band for AP and DA with correlation coefficient more than 0.99. The chromatographic conditions gave compact spots at Rf value (± SD) 0.60 (± 0.011), 0.21 (± 0.01), 0.83 (± 0.01) and 0.08 (± 0.015) for PCT, ACF, AP and DA respectively. The method was validated as per ICH guidelines, demonstrating to be accurate and precise within the corresponding linearity range of analytes. Inherent stability of these drugs was studied by exposing drug substances to stress conditions as per ICH guidelines namely oxidative, thermal, photolysis and hydrolytic conditions under different pH. Relevant degradation was found to take place under these conditions. PCT and ACF were found to undergo extensive acidic and basic hydrolysis while ACF was also susceptible to neutral hydrolysis; producing stated impurities as their major degradation products. The developed method resolved the drugs from degradation products generated under stress conditions; with the peak purity values greater than 0.999. Thus, a new simple, accurate, precise, sensitive and economic stability-indicating High Performance Thin Layer Chromatography (HPTLC)/densitometry method has been developed and validated for the simultaneous estimation of the titled analytes and their stated impurities in pharmaceutical dosage form. The high sensitivity and specificity make it valuable quantitative method suitable to be employed in the routine estimation of impurities and in stability studies.

VALIDATED STABILITY INDICATING HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR REPAGLINIDE API

A simple, precise and accurate stability-indicating high performance thin layer chromatographic method for estimation of repaglinide in bulk drug and in tablet formulation has been developed and validated. The stationary phase used was HPTLC plates precoated with silica gel 60F254 using the mobile phase of chloroform: methanol: ammonia (4.5:1.0:0.05 V/V/V). Densitometric analysis was performed in absorbance mode at 242 nm. The method showed compact bands of drug at RF value of 0.31 ± 0.02. Linear Regression analysis of calibration data showed good linear relationship with r2= 0.9981 in concentration range of 500 - 3000 ng/band. Drug was subjected to ICH-prescribed stress conditions such as acid, base, peroxide, thermal and photolytic degradation and method was found able to separate the peaks for all degradation products from analyte peak. Validation of the developed method was carried out for its specificity, linearity, range, precision, accuracy and robustness. The method was further applied for repaglinide estimation in pharmaceutical tablet formulation and it was found to be reliable. The method was also used successfully to carry out content uniformity test of repaglinide in tablet dosage form.

Stability-Indicating HPTLC Method for Simultaneous Estimation of Flurbiprofen and Chloramphenicol in Ophthalmic Solution.

A specific, accurate and reproducible stability-indicating high performance thin layer chromatography (HPTLC) method was developed for the estimation of flurbiprofen and chloramphenicol in the presence of their degradation products. Degradation studies of both the drugs were carried out in acidic, alkaline, neutral, oxidative, photolytic and thermal stress conditions. Separation was performed on thin layer chromatography plate precoated with silica gel 60 F254 using ethyl acetate : n-hexane : methanol : tri-ethyl amine (5 : 4 : 2 : 0.5, v/v/v/v). Spots at retention factor 0.29 and 0.62 were recognized as flurbiprofen and chloramphenicol, respectively, and were quantified through densitometric measurements at wavelength 267 nm. Method was found to be linear over the concentration range 12-60 ng/spot with correlation coefficient of 0.9997 for flurbiprofen and 200-1,000 ng/spot with correlation coefficient of 0.9977 for chloramphenicol. The proposed method was applied to the estimation of flurbiprofen and chloramphenicol in commercial ophthalmic formulation. The developed HPTLC method can be applied for routine analysis of flurbiprofen and chloramphenicol in the presence of their degradation products in their individual as well as combined pharmaceutical formulations.

Development and Validation of Stability Indicating HPTLC Assay for Determination of Gemifloxacin Mesylate in Dosage Forms

Simple and sensitive stability-indicating high performance thin layer chromatography (HPTLC) assay was developed and validated for quantitative determination of the antibacterial drug, gemifloxacin mesylate (GFX) in presence of its degradation products and ambroxol hydrochloride. The chromatographic separation was performed on HPTLC precoated silica gel plate 60F254 as stationary phase. The mobile phase consisted of a mixture of ethyl acetate: methanol: 25% ammonia, (8:4.5:3, v/v/v). The detection was performed using fluorescence mode and the emission intensity was measured using optical filter K400 after excitation at 342 nm. The Rf value for GFX was 0.47 ± 0.03. Good correlation coefficient was obtained over the concentration range of 1.5 - 180 ng/band. The LOD and LOQ of the proposed method were 0.28 and 0.86 ng/band, respectively. The proposed method was successfully applied for the analysis of GFX in its single and combined dosage forms. Moreover, it was utilized to investigate the kinetics of acidic, alkaline, neutral, oxidative and photolytic degradation of the drug. The apparent kinetic-order rate constants and half-life times of the degradation process were calculated. Furthermore, the proposed method was successfully applied for investigating the factors affecting the storage of GFX.

Stability-indicating High Performance Thin Layer Chromatography /densitometry estimation of Formoterol fumarate dihydrate in bulk and capsules

Novel, simple, rapid and reliable High-Performance Thin-Layer Chromatographic (HPTLC) methods were developed and validated for the analysis of Formoterol Fumarate Dihydrate (FFD) in bulk and in in-house tablet formulation. HPTLC quantitation of FFD was done at UV detection of 281 nm and analysis was performed on (10 cm 10 cm) aluminium sheets precoated with silica gel 60-F 254 (E. Merck) as stationary phase and ethyl acetate: methanol: triethylamine (3.2:1.5:0.3 v/v ) as mobile phase. Quantitation by HPTLC method was performed over the concentration range of 400 - 900 ng/band. The HPTLC method resulted into compact and well resolved band for FFD at retention factor ( R f ) of 0.51 0.3. Linear regression analysis data for calibration of HPTLC method represented good linear relationship with regression coefficient; r 2 = 0.999. The developed methods were validated for precision, robustness, ruggedness, accuracy, sensitivity as per guidelines laid by International Conference on Harmonisation (ICH). FFD was subjected to acid and alkali hydrolysis, oxidation, neutral, photo and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation, and thermal conditions. This indicates that the drug is susceptible to acid, base, oxidation and thermal conditions. The degraded product was well resolved from the pure drug with significantly different R f value. Statistical analysis proved that the developed methods were precise, robust, sensitive and accurate and can be used effectively for the analysis of FFD in bulk and pharmaceutical formulations.

Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of sitagliptin phosphate monohydrate in bulk and in pharmaceutical formulation

Summary A simple, selective, precise, and stability-indicating high-performance thinlayer chromatographic method for analysis of sitagliptin phosphate both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed high-performance thin-layer chromatography (HPTLC) aluminium plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of methanol-water-triethylamine (8:2:0.05 v/v). The system was found to give compact spot for sitagliptin phosphate (Rf value of 0.55 ± 0.03). Densitometric analysis of sitagliptin phosphate was carried out in the absorbance mode at 267 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.998±0.0015 with respect to peak area in the concentration range 1000–6000 ng per spot. The mean value ± SD of slope and intercept was 0.723 ± 0.043 and 17.24 ± 18.78 with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 85.80 and 265.42 ng per spot, respectively. Sitagliptin phosphate was subjected to acid and alkali hydrolysis, oxidation, and photo and thermal degradation. The drug undergoes degradation under acidic, basic, and oxidative conditions. This indicates that the drug is susceptible to acid and base, and oxidation. The degraded product was well resolved from the pure drug with significantly different RF value. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of sitagliptin phosphate in bulk drug and pharmaceutical formulation.

Stability-indicating densitometric high-performance thin-layer chromatographic method for the quantitative analysis of biomarker naringin in the leaves and stems ofRumex vesicariusL.

A simple, sensitive, and stability-indicating high-performance thinlayer chromatography (HPTLC)-densitometric method was developed for the quantification of biomarker naringin in the methanol extracts of stems and leaves of Rumex vesicarius. Chromatography was performed on glass-backed silica gel 60 F254 high-performance thin-layer chromatography (HPTLC) plates with ethyl acetateglacial acetic acid-MeOH-H2O (30:10:5:1, ½/½) as mobile phase. Scanning and quantification were done at 275 nm. The system was found to give compact spot for naringin at RF = 0.46 ± 0.001. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.998 with respect to area in the concentration range of 100–1000 ng. The regression equation of standard was found to be Y = 3.438X + 38.485. Naringin was subjected to acid and alkali hydrolysis, peroxide oxidation, photodegradation, dry heat, moist heat, and ultraviolet (UV) treatment. The drug undergoes complete degradation under acidic tre...

Validated stability-indicating high performance thin layer chromatographic method for determination of Ivabradine hydrochloride in bulk and marketed formulation: An application to kinetic study

A sensitive, selective, precise and accurate stability-indicating high-performance thin layer chromatographic method for analysis of Ivabradine hydrochloride (IH) an anti anginal agent, both as a bulk drug and in formulations was developed and validated according to ICH guideline. Densitometric analysis of IH was carried out in the absorbance mode at 287nm using ethyl acetate: 0.389M ammonium acetate in methanol (1:5, v/v) as solvent system. This system was found to give compact spots for IH at an Rf value of 0.36±0.01. Moreover, IH was subjected to acid and alkali hydrolysis, oxidation, accelerated humidity/temperature, wet heat treatment, and photo degradation. The drug undergoes degradation under mainly acidic and basic conditions. Also the degraded products were well resolved from the pure drug with significantly different Rf values. Linearity was found to be in the range of 1200–2800ng/band. The LOD and LOQ for IH were 255.86ng/band and 775.33ng/band, respectively. “Bartlett’s test” and “Lack of fit” applied on peak area for linearity, additionally proved validity of the developed method. Good accuracy and precision were obtained as revealed from %RSD value less than 2. Similarly, no interference was observed from common excipients in tablet formulation as well as degradation product, indicating specificity of the method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one. Moreover, proposed method was also utilized to investigate the kinetics of acidic degradation process at different temperatures and first order rate constant, half-life, shelf-life and activation energy were calculated.

Stability Indicating HPTLC Method for Estimation of Modafinil in the Bulk and Tablet Formulation

A simple, selective, precise and stability-indicating high-performance thin layer chromatographic method for analysis of Modafinil, both as the bulk drug and in a tablet formulation has been developed and validated. Aluminum foil TLC plates precoated with silica gel 60F 254 were used as stationary phase ethyl acetate, acetone and methanol in the volume ratio of (7:2:1 v/v) respectively as mobile phase. A compact band (Rf 0.42±0.02) was obtained for modafinil. Densitometric analysis was performed in absorbance mode at 232 nm. Linear regression analysis revealed a good linear relationship (r 2 =0.9995) between peak area and concentration in the range of 80-320 ng /spot. The method was validated for precision, recovery, and robustness. The limits of detection and quantitation were 15 and 50 ng/spot, respectively. Modafinil was subjected to acid and alkaline hydrolysis, oxidation, photochemical and thermal degradation and underwent degradation under all these conditions. Statistical analysis proved the method enables repeatable, selective, and accurate analysis of the drug. It can be used for identification and quantitative analysis of Modafinil in the bulk drug and in tablet formulations.

Development and validation of HPTLC method for the estimation of diosgenin inIn Vitroculture and rhizome ofDioscorea deltoidea

Summary A new simple, accurate, selective, precise, economical and stability-indicating high-performance thin layer chromatographic method for the analysis of diosgenin in callus and rhizome of Dioscorea deltoidea was developed and validated. The method was developed on TLC aluminium plates precoated with silica gel 60F254 using solvent system petroleum ether-isopropanol (12:1, v/v), which gives a compact spot of diosgenin (RF value 0.76 ± 0.02). Densitometric analysis of diosgenin was carried out in the absorbance mode at 366 nm after spraying with methanolic sulphuric acid. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.991 and 0.995 for diosgenin with respect to peak height and peak area, respectively, in the concentration range of 100–1000 ng per spot. The limits of detection and quantification for diosgenin were 16.58 and 50.25 ng per spot. The proposed method was applied for determination of diosgenin in rhizome of D. deltoidea (0.047% w/w) ...

APPLICATION OF STABILITY INDICATING HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC METHOD FOR QUANTITATION OF DESVENLAFAXINE IN PHARMACEUTICAL DOSAGE FORM

This paper describes a sensitive, selective, precise, and stability-indicating high performance thin layer chromatographic method for the determination of desvenlafaxine both as a bulk drug and in formulation. The method uses aluminum plates precoated with silica gel 60F-254 as the stationary phase and solvent system ethyl acetate:toluene:methanol:ammonia 7:2:0.5:0.5, (v/v/v/v). This system gave compact spots for desvenlafaxine (0.48 ± 0.06). Desvenlafaxine 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 R f values. Densitometric analysis of desvenlafaxine was performed in the absorbance mode at 228 nm. The linear regression analysis data for the calibration plots showed a good linear relationship over concentration range of 100–1000 ng · spot−1. The mean values of the correlation coefficient, slope, and intercept were 0.9997 ± 0.04, 7.4521 ± 0.437, and 781.15 ± 0.51, respectively. The method was validated for precision, robustness, and recovery. The limit of detection and limit of quantitation were 10 and 100 ng · spot−1, respectively. Statistical analysis showed that the method is repeatable, selective, and can separate the drug from its degradation products and can be used to monitor stability.