Silica Gel GF254 Research Articles

HPTLC method for determination of anti-hypertensive drug combination metoprolol succinate and dapagliflozin

Combination of Metoprolol Succinate and Dapagliflozin is recommended in the treatment of Hypertension. Accurate and precise thin layer chromatographic method has been developed for the determination of Metoprolol Succinate and Dapagliflozin in combination. Pre-coated silica gel G60—F254 aluminium sheet (10 × 10 cm),0.2 mm layer thickness used as stationary phase and n-Butanol: Ethyl acetate: Triethylamine (6:4:0.1 v/v/v) used as mobile phase. The method was found to be linear with a range of 200–1200 ng/band for DAP and 1000–6000 ng/band for MET with correlation coefficient (r2) 0.996 for both DAP and MET. The proposed method was validated as per ICH Q2 (R2) guideline with respect to linearity, accuracy and precision. Stress degradation was carried out to find out the intrinsic stability of the molecules. Both the drugs were highly susceptible to acid and base hydrolysis and degradation products were well separated with drug peak. The method was successfully used for determination of metoprolol succinate and dapagliflozin in combination.

A validated HPTLC method for quantification of a new combination containing Lidocaine HCl and Diltiazem HCl

Regulators approve newer medications and medication combinations for the treatment of various disorders. For the treatment of anal fissures, a novel combination of currently available medications, such as lidocaine HCl and diltiazem HCl, has been approved. The current work represents high-performance thin layer chromatographic method to estimate the amounts of lidocaine hydrochloride and diltiazem hydrochloride in a combined gel dosage form called Crema-L gel (2% W/W of lidocaine and 2% W/W of diltiazem hydrochloride). This method has been validated. The mobile phase in this method consisted of a mixture of toluene, methanol, ethyl acetate (7:2: 1% v/v/v) and two drops of ammonia. The stationary phase was pre-coated aluminium sheet with silica gel G60 F254 (10 × 10 cm, 0.2 mm layer thickness). The drugs’ resolved peaks were found at the Rf values of 0.59 for Lidocaine HCl and 0.48 for Diltiazem HCl. The overlay UV spectra of the two medications were used to determine the analytical wavelength and at 220 nm, both drugs showed appreciable absorbance. The concentration range of 400–1200 ng/band was determined to be the linear approach for both lidocaine HCl and diltiazem HCl, as indicated by their respective correlation coefficients (r2) of 0.9987 and 0.9980. The technique for simultaneously estimating lidocaine hydrochloride and diltiazem hydrochloride in bulk and pharmaceutical dosage form was shown to be robust, accurate, precise, and repeatable.Graphical

Development and Validation of HPTLC for the Determination of Gefitinib HCl in Tablet Dosage Form

A simple, high-performance thin-layer chromatography (HPTLC) method of gefitinib HCl in pharmaceutical formulation was developed. Separation was done on TLC aluminum plates precoated by silica gel 60GF254 (20 × 20 cm) with 200 μm layer depth. With UV detection set to 254nm, chromatography was conceded out by the mobile phase of dichloromethane and methanol (9:1, v/v). Linearity was found to range of 50 to 300 ng/spot and, the correlation coefficient was found to be 0.99 and the Rf value was found to be 0.46. The system’s suitability was considered to ascertain the performance of ascertaining quality performance of the developed chromatographic method. The method’s accuracy, precision, and specificity were all verified against the International Council of Harmonization (ICH) standards. Application of the approach to the determination of gefitinib in tablet form was successful.

Identification of Medicinal Chemicals (BKO) Piroxicam in Jamu Pegal Linu Preparations in Makassar City

The aim of the research was to identify Piroxicam in herbal medicine for rheumatic pain circulating in Makassar. There are several traditional medicines that contain medicinal chemicals. Research has been conducted on the identification of medicinal chemicals (BKO) on several rheumatic herbs preparations in herbs shops in Makassar. The BKO which is often included in rheumatic herbs is the NSAID group, one of which is piroxicam. This inspection was conducted to know the presence of the chemical drug piroxicam contained within rheumatic herbs preparations and the samples used were 5 samples. The method used was a qualitative test using thin layer chromatography (TLC) consisting of a mobile phase mixed with n-hexane and acetone (7:3) and a stationary phase using Silica Gel GF254. The results of the TLC examination from 5 samples of herbal medicine added BKO piroxicam contained 3 samples including herbs A, B, and C because they had the same stain color at the same Rf value as the piroxicam. Some of the rheumatic herbs circulating in Makassar contain medicinal chemicals in the form of piroxicam.

IDENTIFICATION OF MEDICINAL COMPOUND IN URIC ACID JAMU BY THIN LAYER CHROMATOGRAPHY METHOD

Jamu is one of the traditional medicines derived from natural ingredients distributing in Indonesia. In accordance with Permenkes No. 007 of 2012, Medicinal Compound (MC) are prohibited from being added to jamu products. Previous research has found that some of the products in public contain MC. The aim of this study is to determine the presence or absence of allopurinol, piroxicam, and dexamethasone in uric acid jamu. This research used 5 (five) samples of uric acid jamu, both those with and without distribution permits from The Indonesian Food and Drug Authority, randomly selected in Kedawung District, Cirebon Regency, West java, Indonesia. The identification method used in this study is Thin Layer Chromatography (TLC) with the stationary phase being silica gel GF 254. For the identification of allopurinol, the mobile phase is n-butanol: ammonium hydroxide: ethanol; for piroxicam identification, it is ethyl acetate-methanol-ammonia (6:3:1); and for dexamethasone identification, it is chloroform: acetone (1:4). Spot detection is done using ultraviolet (UV) light at 254 nm. The applied solutions are the test solution (A), the test solution with added allopurinol, piroxicam, or dexamethasone (B), and the reference standard solution (C). The research results from the 5 (five) samples of uric acid jamu identified one positive samples containing allopurinol, and all positive samples contained piroxicam and dexamethasone. Keywords: Jamu, thin-layer chromatography, allopurinol, piroxicam, dexamethasone

Development and validation of stability indicating high‐performance thin‐layer chromatographic method for estimation of Rifapentine in pharmaceutical formulation

AbstractA simple, accurate, and precise method is described for stability indicating a high‐performance thin‐layer chromatographic (HPTLC) method for development and validation in the pharmaceutical dosage form. The method was based on HPTLC separation of the drug by measurement of the spot at 478 nm. Separation was carried out on silica gel 60GF254 by using mobile phase methanol:toluene:acetic acid (3:7:0.1, v/v/v). The linearity range was between 500–3000 ng/spot with a coefficient of determination 0.999, respectively. The retardation value found was 0.55 ± 0.02 and the % recovery was found to be 100.610 ± 0.035%–101.0178 ± 0.035%. The limit of detection value for Rifapentine was 92.901 ng/spot and the limit of quantitation for Rifapentine was found to be 281.52 ng/spot. Forced degradation studies were carried out under various conditions. In acidic conditions, the % degradation was found to be 20.07%. In alkaline and oxidative conditions, the % degradation was found to be 61.27% and 11.12%. Photolytic and thermal conditions the % degradation was found to be 49.75% and 8.35%. Maximum degradation was found in alkaline condition with 61.27%, an assay for the marketed formulation was carried out and the amount of drug was found to be 149 ± 0.05 mg with a % of 99.25% ± 0.005%.

Derivatization-Based Novel Chromatographic and Spectrophotometric Methods for the Simultaneous Determination of Gymnemic Acid and Resveratrol in Antidiabetic Polyherbal Formulation.

Herbal medicine is widely used for the treatment and prevention of various ailments, highlighting the importance of ensuring its consistency and quality. This research focuses on the simultaneous detection of Gymnemic acid (GYM) and Resveratrol (RES) in an antidiabetic polyherbal formulation as no reported method exists for their simultaneously detection. The objective of this study is to develop and validate novel derivatization-based spectrometric and HPTLC methods for the simultaneous determination of GYM and RES. The spectrophotometric method involved derivatization of GYM with benzoyl chloride, followed by measurement of absorbance at 349nm an isoabsorptive point. The HPTLC method utilized post derivatization with vanillin-sulfuric acid, and its separation was achieved on pre-coated silica gel 60GF254 using chloroform:methanol:glacial acetic acid (13:4:0.1, v/v/v) as mobile phase and estimated at 575nm. The developed method exhibits linearity, accuracy, precision, LOD, LOQ, specificity and robustness in accordance with the ICH Q2 (R1) guideline. The percent assay of GYM and RES in the marketed capsule formulation was statistically compared using an unpaired t-test, resulting in a range of 99.51-102.65%. These indicate no significant difference between the proposed method and the marketed formulation. Therefore, both novel methods can be interchangeably used for quality control of GYM and RES in polyherbal formulations.

Establishment of Thin Layer Chromatographic Fingerprints for the Quality Control of Chanthalila Preparation, A Thai Traditional Antipyretic Medicine

Objective: This study aimed to develop thin layer chromatographic (TLC) fingerprints to control the quality of Chanthalila preparation (CP).Material and Methods: Twelve batches of reference CP were prepared from various sources and used as reference batches (CP1 to CP12). Artemisinin, atractylodin, eurycomanone, imperatorin and loureirin A were used as markers. The common and characteristic bands were assigned using the reference TLC fingerprints and applied to assess the qualitative parameters used in the identification and chemical profiling of eight commercial CPs.Results: The reference TLC fingerprints were established on a silica gel GF254 plate with two mobile phase systems, System A and System B. In System A, atractylodin, imperatorin, and loureirin A were assigned as characteristic bands along with 10-12 common bands under Ultraviolet (UV) 254 nm, UV 366 nanometer (nm), and derivatization. In System B, 6 common bands were observed under UV 254 nm, while 11 fluorescent bands were detected under UV 366 nm. Eurycomanone and artemisinin were not found in any reference CP batches, which revealed the TLC method had poor sensitivity. The TLC patterns of commercial CPs were markedly different from those of the reference fingerprints. Most commercial products failed to meet the specification criteria because only imperatorin appeared in the chromatogram.Conclusion: TLC fingerprinting is a fast and efficient method that can be employed in the quality control of CP. It enables the revelation of the quality of the raw materials in the chromatograms, which can be useful to manufacturers to evaluate their supplier sources. However, the sensitivity of this method for determining some markers was quite low.

HPTLC Method Development and Validation for the Simultaneous Estimation of Nortriptyline HCl and Pregabalin in their Combined Dosage Form.

Nortriptyline HCl and pregabalin Tablet is used to treat neuropathic pain as well as mental or mood issues such as sadness, mood, feelings, anxiety and tensions. Very few analytical methods are available for the simultaneous estimation of nortriptyline HCl and pregabalin and no reports has been found for HPTLC method. In the current study, a reliable HPTLC method for the simultaneous measurement of nortriptyline HCl and pregabalin in pure forms and pharmaceutical formulations has been developed with ninhydrine post derivatization of pregabalin. The HPTLC method development was carried using silica gel G60 F254 as stationary phase and acetonitrile: methanol: triethylamine: water: formic acid (7:3:0.3:0.8:0.02v/v/v/v/v) was used as mobile phase with saturation time of 20min. The system was found to give a compact band for nortriptyline HCl (Rf = 0.523 ± 0.008) pregabalin (Rf = 0.279 ± 0.005). The developed method was found to be validated as per ICH Q2 (R1) guideline. The peak of nortriptyline HCl and pregabalin showed good linearity over the concentration range of 50-300ng/band and 350-2250ng/band, respectively, with a correlation coefficient of ˃0.995. The % recoveries of both drugs were found to be in the range of 98.84-101.87%. Statistical analysis proved that the method is selective, precise, robust and accurate for the estimation of nortriptyline HCl and pregabalin.

Detection of synthetic lipid‐lowering adulterants in herbal products using high‐performance thin‐layer chromatography

AbstractAdulterating herbal medicine with undeclared synthetic drugs is a worldwide problem that seriously threatens human health. To detect such illicit and not labeled synthetic hypolipidemic substances in herbal medicines, an analytical method to simultaneously identify and quantify atorvastatin (ATV) calcium, simvastatin (SIM), gemfibrozil (GEM), fenofibrate (FEN) belonging to two different classes of drugs (statins and fibrates) was developed based on high‐performance thin‐layer chromatography. The method consisted of Silica Gel G60 F254 precoated aluminum plate as stationary phase and toluene: ethyl acetate: formic acid (7:3:0.3, v/v/v) as optimized mobile phase. The densitometric evaluation wavelength was optimized at 254 nm. The Rf values of ATV, SIM, GEM, and FEN were 0.157, 0.268, 0.691, and 0.852, respectively. The linearity range is between 100–1500 ng/band for ATV and FEN and 200–3000 ng/band for SIM and GEM, respectively. The accuracy was found to be in the range of 97%–105%. The relative standard deviation of precision and robustness was found to be < 5%. However, the five screened market samples did not show the presence of adulteration of the above drugs. This method for the simultaneous determination of four drugs may be successfully employed to screen synthetic hypolipidemics as adulterants in herbal products and dietary supplements.

Analytical Quality Risk Assessment and Design of Experiments to Green HPTLC Method for Simultaneous Estimation of Sildenafil Citrate and Dapoxetine Hydrochloride.

A green and robust high-performance thin-layer chromatographic method has been developed for the simultaneous estimation of sildenafil citrate and dapoxetine hydrochloride. A fractional factorial design was applied for analytical quality risk assessment of potential analytical risk factors. The identified critical analytical risk factors were optimized using the design of experiment-based response surface analysis by full factorial design. The analytical design space was navigated for the optimization of the method and the control strategy was framed for low-risk life-cycle management of the chromatographic method. The chromatographic analysis of sildenafil and dapoxetine was carried out on a TLC plate coated with silica gel G60 F254 using n-butanol:ethyl acetate:ethanol (8.0 + 2.0 + 0.5, v/v) as mobile phase. The chromatographic peaks of sildenafil and dapoxetine were found to be at Rf 0.29 and 0.69, respectively. The method was found to be accurate, precise, robust, specific and sensitive. The fixed-dose combinations of sildenafil and dapoxetine were assayed and results were found in compliance with their labeled claim. The present method was developed using safe and eco-friendly organic solvents for the safety of analysts and the protection of the environment. The greenness profiles of developed and reported methods were evaluated using the NEMI scale and AGREE software.

Comparative Pharmacognostical Evaluation and HPTLC Analysis of Stem Bark of Kanchnar (Bauhinia Variegata Linn.) and Kovidar (Bauhinia Purpurea Linn.)

The current study was carried out to provide comparative macroscopy, microscopy, physicochemical parameters and HPTLC analysis of stem bark of Kanchnar (Bauhinia variegata L.) and Kovidar (Bauhinia purpurea L.) T.S. of stem bark of Bauhinia variegata L. shows a wide stratified cork have thin-walled yellow brown cells followed by brown colored cells; inner cork layer has transversely elongated orange brown cells. T.S. of Bauhinia purpurea L of shows presence of few layers of cork, Outer layers contains reddish brown content and inner layers are colourless. Its cortex is composed of 10 to 12 layers of parenchyma cell. Total Ash value found in sample of Kanchnar was 5.67% and in Kovidar was 15.2%. The Alcohol soluble extractive value of Kanchnar was found 29.8 % and of Kovidar was found 4.8%. Water soluble extractive value in sample of Kanchnar was found 20.68% and in Kovidar it was found 13.83%. Reference marker betasitosterol and lupeol was applied on a pre-coated silica gel GF254 plate of uniform thickness (0.2mm). The mobile phase consisting Toluene: Ethyl acetate: formic acid (9:1:0.1). Presence of marker betasitosterol and lupeol in sample of Bauhinia variegata L. were 85.19µg/ml and146.4µg/ml respectively. Presence of marker betasitosterol and lupeol in sample of Bauhinia purpurea L. were 244.6µg/ml and 305µg/ml respectively.

Identification of Paracetamol and Caffeine in Jamu Powders Simultaneously Using TLC-Densitometry

Paracetamol and caffeine are chemical compounds that are suspected to be illegally added to the traditional herbs claimed as rheumatics drugs. Identification of paracetamol and caffeine has been done on five samples of jamu powder obtained from the Depot Jamu in Surabaya. This study aimed to simultaneously identify paracetamol and caffeine commonly found in traditional medicine one of which is jamu powder using thin-layer chromatography densitometry (TLC-Densitometry). Evaluate the presence of paracetamol and caffeine in the product of jamu was performed by thin layer chromatography with silica gel GF254 and chloroform-ethyl acetate (1:1) as the stationary and mobile phase respectively. The spots on the TLC plate were detected using a UV at 254 nm and the areas were measured by a Camag TLC scanner. The TLC profile demonstrated a good separation of paracetamol, caffein, and others substances that containing in the products. The retardation factor (Rf) of paracetamol and caffeine were 0,42 and 0,26 with a detection limit of 0,0125 µg/spot and 0,05 µg/spot respectively. The simultaneous identification of caffeine and paracetamol by using thin-layer chromatography densitometry revealed that none of the five samples were detected to contain paracetamol and caffeine. Keywords: Simultaneously, Identification, Paracetamol, Caffeine, Jamu Powder, TLC- Densitometry

In-vitro Sun Protecting Factor of Rice Bran Oil and Its Formulation as Compact Powder

This study aims to determine the effective concentration of rice bran oil which can protect against ultraviolet (UV) rays as well as formulate it in compact powder preparation followed by determination of its Sun Protecting Factor (SPF) value. Rice bran samples were extracted using the Soxhlet extraction method with n-hexane: ethanol (1:1) as the solvent. Further identification of the γ-oryzanol in rice bran oil was carried out using TLC silica gel GF254 with eluent of n-hexane:ethyl acetate (3:1). The obtained γ-oryzanol in rice bran oil was used as the ingredient to develop the compact powder which is made into five formulas with 0,05 %-0,25 % concentration. All formulas were characterized, including homogeneity, adhesion and crack test. UV-Visible spectrophotometry was used to determine the SPF value of rice bran oil and its compact powder. The identification results demonstrated a positive presence of the chemical γ-oryzanol in the rice bran oil. At concentrations of 500, 1000, 1500, 2000, and 2500 ppm, rice bran oil may protect against UV rays with SPF values ranging from 1.741 to 11.884. The result showed that all formulas dispersed homogeneously, performed well in terms of compactness, and had no breaks or cracks discovered. Meanwhile, the SPF values of all formulas are found to be 1.390 and 1.274. The results indicate that the SPF values are shallow and are included in the minimal SPF category (2-4) in protecting against UV rays.

Stability-Indicating HPTLC Method for Determination of Remogliflozin Etabonate and Vildagliptin in Tablets.

A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method is developed for the simultaneous estimation of remogliflozin etabonate and vildagliptin in the presence of their degradation products. The separation was performed in thin layer chromatography plate precoated with silica gel G60F254. The mobile phase consists of methanol:ethyl acetate:toluene:ammonia (1.5:4:4.5:0.1, v/v/v/v). Detection and quantification are performed with densitometer at 212nm. The Rf values of remogliflozin etabonate and vildagliptin are 0.53 and 0.42, respectively. Degradation studies for the two drugs were carried out in acidic, alkaline, neutral, oxidative, photolytic and thermal stress conditions and analyzed. The suitability of this method for the quantitative determination of the compounds is proved by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH). Linearity was found over the concentration range of 200-1000ng/band with correlation coefficient of 0.9936 for remogliflozin etabonate and 100-500ng/band with correlation coefficient of 0.9912 for vildagliptin. The method was successively applied to tablets containing two drugs and found to have no chromatographic interferences from the tablet excipients. The degradant formed was not interfering with estimation of two drugs makes the method more selective for the purpose intended.

ANTIBACTERIAL ACTIVITY AND BIOAUTOGRAPHIC EVALUATION OF EXTRACT AND FRACTION FROM TAMOENJU (HIBISCUS SURATTENSIS L.) LEAVES

Objective: The tamoenju (Hibiscus surattensis L.) is one of the plants as traditional medicines to treat infections. Tamoenju leaves contain alkaloids, flavonoids, saponins, tannins, and steroids, a potential antibacterial agent. This study aimed to determine the antibacterial activity of tamoenju leaves extract and fraction against Staphylococcus aureus (ATCC 25923) and Salmonella typhi (ATCC 14028), and detect the active compounds using Thin Layer Chromatography (TLC) Bioautography techniques.
 Methods: The sample was extracted using maceration method with 96% ethanol as solvent. Fractionation of ethanol extract using the liquid-liquid extraction method using n-hexane and ethyl acetate. The agar well diffusion method was used to evaluate the antibacterial activity with various concentrations of 2.5%, 5%, 10%, and 20%, followed by TLC bioautography using n-butanol: acetic acid: aquadest (4:1:1) as the mobile phase and silica gel GF 254 as the stationary phase on the most active fraction. Zones of inhibition showed the sensitivity of the tested microorganisms.
 Results: The results showed the extract, n-hexane, and water fractions were more sensitive to S. typhi, while the ethyl acetate fraction was more sensitive to both bacteria. The zone of inhibition increased with the increasing extract and fractions concentration. The bioautography TLC showed that the compounds that had the potential as antibacterial in the most active fraction (ethyl acetate fraction) were flavonoids.
 Conclusion: The extract and fraction of tamoenju leaves have antibacterial activity. Ethyl acetate fraction had the highest antibacterial activity. The compounds predicted to have antibacterial activity against the two tested bacteria were flavonoids.

Simultaneous quantification of pharmacological markers quercetin, berberine HCl and curcumin using High-performance thin-layer chromatography (HPTLC) from polyherbal formulation

Quercetin, curcumin and berberine HCl have anti-acne, antimicrobial, anti-inflammatory, antioxidant properties. In the present study an attempt has been made to develop a simple, precise, rapid, selective and cost-effective high-performance thin-layer chromatographic (HPTLC) method for simultaneous estimation of quercetin, curcumin and berberine HCl from polyherbal gel prepared for the treatment of Acne. The method was developed using HPTLC silica gel GF254 precoated aluminium plate as a stationary phase. The solvent system consisted of Toluene, Ethyl acetate, Methanol, Formic acid. Densitometric analysis was carried out in the absorbance mode at 254nm. This system was found to give compact spots for quercetin, curcumin and berberine HCl at specific Rf values. The linearity of quercetin, curcumin and berberine HCl were obtained between 200 and 1000 ng/spot with good correlation coefficient values. The % of quercetin, curcumin and berberine HCl from polyherbal gel was found to be 99.42±0.98, 98.67±0.76% and 99.6±1.06% respectively, which was well within the limit. It was concluded that the developed HPTLC method would be an important tool in the quality control of polyherbal formulations.

STANDARDIZATION OF SECONDARY METABOLITES AND HEAVY METAL CONTAMINATION ASSAY ON ONCHIDIID SLUG (ONCHIDIUM TYPHAE) WEST KALIMANTAN WATERS

Onchidiid slug or Onchidium typhae is a marine animal commonly found in West Kalimantan waters. This gastropod is commonly used as medicine and cosmetic by the locals. This research aims to assure the content and quality of O. typhae methanol extract by determining its secondary metabolites and heavy metal contamination. Phytochemical screening of alkaloid, steroid/ triterpenoid, flavonoid, tannin, and saponin are done using reagent tests. Chromatography profile was completed using silica gel G60 F254 plate and hexane: ethyl acetate: methanol as mobile phase. Heavy metal contamination analysis was performed using atomic absorption spectrophotometry to determine Hg, As, Cd, and Pb content. The phytochemical screening and chromatography profile of O. typhae methanol extract confirm the presence of alkaloids and steroids. Heavy metal analysis stated Hg, As, Cd, and Pb content in O. typhae are < 0,0008; < 0,001; < 0,001; and 0,05 ppm respectively. Since heavy metal levels are below the maximum contamination limit, it qualifies as a natural product ingredient.

High-Performance Thin Layer Chromatography Method for Simultaneous Estimation of Water-Soluble Vitamins: Analytical Method Development, Validation and Applications

Vitamins are pivotal ingredients in dietary supplements and nutraceutical products. Since many vitamins are unstable and rapidly degraded, it’s crucial to keep track of their loss throughout processing and storage. Monitoring hydrophilic vitamins may be more crucial than monitoring those lipophilic vitamins because the body does not maintain them as well. There seems to be a need for an all-encompassing method to estimate hydrophilic vitamins. In this study, we have developed a high-performance thin layer chromatography method for estimation of four water-soluble vitamins simultaneously using HPTLC silica-gel 60GF254 plates and ethyl acetate: methanol: hydrochloric acid (0.1N) (8.5:1:0.5 v/v/v) as a mobile phase, which was successfully validated as per the ICH guideline. All the validation parameters were within the acceptable range established by the ICH guideline. The method is precise, reproducible, easy, reliable, and applicable for the estimation of water-soluble vitamins in marketed products. To best of our knowledge, it is simpler, less time-consuming, and more economical than other approaches that have been published for the same purposes

Chemometric-Based AQbD and Green Chemistry Approaches to Chromatographic Analysis of Remogliflozin Etabonate and Vildagliptin.

According to the green chemistry approach, during method development, the usage of toxic and carcinogenic organic solvents should be avoided or minimized for the safety of the environment and analysts. The chromatographic methods such as reverse-phase high-pressure liquid chromatography (RP-HPLC) and high-performance thin-layer chromatography (HPTLC) include the usage of class 2 organic solvents as per the International Council for Harmonization (ICH) Q3C (R6) guideline. The chromatographic analysis by HPTLC requires less organic solvent compared to the RP-HPLC method. Hence, HPTLC-based chromatographic analysis of vildagliptin (VIL) and remogliflozin etabonate (RMG) has been carried out using green chemistry and analytical quality by design (AQbD) approaches. The principal component analysis (PCA)-based chemometric analysis was applied for the identification of critical method variables (CMV) for the development of the method. The design of experiments (DoE)-based Box-Behnken design (BBD) was applied for response surface modeling (RSM) and optimization of CMV. The analytical design space (ADS) and analytical control point were navigated for the development of the HPTLC method as per the quality target analytical profile. The chromatographic analysis of VIL and RMG was carried out using silica gel G60 F254 as the stationary phase and acetone-ethyl acetate-water-triethylamine (7.0 + 2.5 + 0.3 + 0.2, v/v) as the mobile phase. The HPTLC method was validated as per the ICH Q2 (R1) guideline. The HPTLC method was applied for the assay of fixed-dose combinations (FDCs) of VIL and RMG, and the results were found to comply with their labeled claim. The developed method included the usage of organic solvents that belong to the class 3 category as per the ICH Q3C (R6) guideline. Hence, the developed method can be used as an eco-friendly alternative to published chromatographic methods for quality control and routine analysis of FDCs of VIL and RMG in the pharmaceutical industry. Chromatographic analysis of VIL and RMG using green chemistry and AQbD approaches. Application of the method for assay of drugs in their combined pharmaceutical dosage forms.