Usmangani K Chhalotiya
@iicp-cvm.edu.in
Associate Professor, Department of Pharmaceutical Chemistry and Analysis
Indukaka Ipcowala College of Pharmacy
EDUCATION
M. Pharm, Ph D
RESEARCH INTERESTS
Keen interest in the Development and Validation new Analytical Methods on sophisticated Instruments like UV – Visible Spectroscopy, High performance Liquid
Chromatography (HPLC), High performance thin layer chromatography (HPTLC) etc., Forced Degradation studies and Impurity Profiling
Scopus Publications
Scopus Publications
Rutvik Pandya, Heta M. Kachhiya, Dhaval Solanki, Jinal Tandel, Usmangani Chhalotiya, and Dimal Shah
Wiley
AbstractAnemia with chronic kidney disease treating newer hope is recently approved Desidustat. By following International Conference on Harmonization Quality guideline Q2 (R1), an economic high‐performance thin‐layer chromatography method has been developed for the estimation of Desidustat. Pre‐coated silica gel 60 F254 plates as stationary phase along with mobile phase toluene:methanol:glacial acetic acid (7.5:2.5:0.3 v/v/v), and 230 nm detection wavelength was selected as optimized. Developed method was found linear in quantity per band range of 100 ng/band to 600 ng/band for Desidustat with 0.9979 regression coefficient. Standard spiking method showed method accuracy with a mean percentage recovery of 99.21%–101.63%. Limit of detection and limit of quantitation were found to be 3.94 and 11.94 ng/band, respectively. The method was found to be linear, precise, accurate, robust, rugged, selective, sensitive, and specific for the quantification of Desidustat in bulk and tablet dosage form and successfully can be applied for the qualitative and quantitative determination of Desidustat in bulk and marketed tablet formulation.
Hetaben Kachhiya, Rutvik Pandya, Krunal Solanki, Jinal Tandel, Usmangani Chhalotiya, and Dimal Shah
ACG Publications
: The hypoxia inducible factor prolyl hydroxylase inhibitor Desidustat is used to treat anemia linked to chronic kidney disease (CKD). For the estimation of Desidustat in bulk and commercial tablet formulation known as Oxemia, a precise, accurate, and sensitive reverse phase HPLC method has been developed and validated. The method described here was optimised with a Hypersil C18 (250 × 4.6 mm, 5 µm) column serving as the stationary phase and a mobile phase that included methanol: acetonitrile (80:20 v/v) added to the column at a flow rate of 1 mL/min. Using a photo diode array detector, Desidustat was detected at an analytical wavelength of 230 nm. With a correlation coefficient of 0.9989, the developed method was found to be linear in the concentration range of 1–6 µg/mL. Every parameter listed in the in International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Quality 2 (Revision 1) guideline was verified for the described method.
Mansi Patel, Usmangani K Chhalotiya, Dimal A Shah, Jinal N Tandel, and Hetaben M Kachhiya
Wiley
Dhavalsinh P. Solanki, Vishal R. Panday, Dimal A. Shah, Usmangani Chhalotiya, Jinal N. Tandel, and Heta M. Kacchiya
Wiley
Dhavalsinh P. Solanki, Krunal H. Solanki, Jaineel V. Desai, Dimal A. Shah, and Usmangani K. Chhalotiya
Informa UK Limited
Abstract A combination of Azilsartan Medoxomil and Cilnidipine is prescribed in the treatment of Hypertension. The present work represents an accurate and precise high-performance thin layer chromatographic method for the estimation of Azilsartan Medoxomil (AZL) and Cilnidipine (CLN) in combined tablet dosage form. Pre-coated silica gel- G60 F254 aluminum sheet (100 × 100 mm, 0.2 mm layer thickness) were used as stationary phase and Ethyl Acetate: Toluene: Glacial Acetic Acid (5: 4.9: 0.1 %v/v/v) in the mixture was used as mobile phase. The method was linear in the concentration range of 200 - 2000 ng/band for AZL and 50 -500 ng/band for CLN with a correlation coefficient (r2) of 0.996 for AZL and 0.999 for CLN. The proposed method was validated with respect to linearity, accuracy, precision, and robustness as per ICH Q2 (R1) guideline. A forced degradation study was performed to assess the stability indicating the nature of the method. All the degradant peaks were well resolved from the peak of the drug without any interference. The method was successfully applied for the analysis of AZL and CLN in combined tablet formulation. GRAPHICAL ABSTRACT
Mansi M. Patel, Usmangani K. Chhalotiya, Dimal A. Shah, Hetaben M Kachhiya, and Jinal N. Tandel
Wiley
Shifa Vahora, Usmangani K. Chhalotiya, Hetaben Kachhiya, Jinal Tandel, and Dimal Shah
Springer Science and Business Media LLC
J. Patel, Jinal N. Tandel, U. Chhalotiya and Kirtan Patel
International Society of Communication and Development Between Universities (ISCDBU)
Alopecia areata is a typical non-scarring alopecia that happens in 0.1-0.2% of everybody and records for 0.7-3% of all cases found in dermatology practice. A vital quantitative examination of Minoxidil and Finasteride was created in Bulk and pharmaceutical measurement structure with precise, and sensitive stability indicating high performance thin layer chromatographic (HPTLC) technique. The chromatographic improvement was done on the HPTLC plates precoated with silica gel 60 F254 utilizing a mobile phase of n-butanol: TEA (10:0.1v/v) as versatile stage. Detection was completed densitometrically at 223 nm. The Rf estimation of medication was seen as 0.22 ± 0.24 for Minoxidil and 0.63 ± 0.65 for Finasteride. The technique was approved according to the ICH rule concerning linearity, accuracy, precision and robustness. The calibration curve was seen as straight over a scope of 6000-24000 ng/band for Minoxidil and 200-800 ng/band for Finasteride with a regression coefficient of 0.9972 For Minoxidil and 0.998 for finasteride. The % recovery was found 98-101.92% for Minoxidil and 98.42-101.68% for Finasteride. Forced degradation studies like acid hydrolysis, base hydrolysis, oxidation, dry heat and photolytic degradation were performed. The degradation products obtained were well resolved from the pure drugs with significantly different Rf values. The proposed technique could viably isolate the medications from its degradation products just as from excipients. The proposed TLC technique has expected subjective just as quantitative applications for synchronous estimation of minoxidil and finasteride in bulk and pharmaceutical dosage form.
Dimal A. Shah, Jesheeka M. Patel, Ashok Mahajan, and Usmangani Chhalotiya
Wiley
Dimal A. Shah, Pankti A. Patel, and Usmangani Chhalotiya
Springer Science and Business Media LLC
Veena S Patel, Usmangani K Chhalotiya, Sandip B Patel, and Jivani Nuruddin
Oxford University Press (OUP)
Abstract Background Liquid chromatography with tandem mass spectrometry is used widely used for the quantitative analysis of phytoconstituents present in medicinal plants to assess the quality of extract used for different investigations. Objective A sensitive, precise, and accurate liquid chromatographic method with tandem mass spectrometric detection was developed for simultaneous quantification of lupeol, betulinic acid, and β-sitosterol in the methanolic extract of Madhuca longifolia bark. Method The three compounds were eluted with a stationary phase Gemini C18 column (50 × 2.0 mm, 3 μm id) and the temperature of the column was maintained by a column oven at 40 ± 0.3°C; mobile phase A (water and 0.1% formic acid) and mobile phase B [acetonitrile–methanol (50+50, v/v) and 0.1% formic acid] were used in a gradient mode and the flow rate was 0.4 mL/min. Results With these conditions, the retention time for betulinic acid, lupeol, and β-sitosterol was found to be 1.25, 3.08, and 3.53 minutes, respectively. The total run time was 5.0 min. Detection and quantitation of all three phytoconstituents were carried out by the mass spectrometer, a triple quadrupole equipped with atmospheric pressure chemical ionization, and multiple reaction monitoring using the predominantly positive ion mode and obtained much higher and more stable response nebulizer gas flow at 3.0 L/min. Linear responses were exhibited for all three phytoconstituents with a dynamic linear range of 10–100 μg/mL with the values of the regression coefficient more than 0.995 for betulinic acid, lupeol, and β-sitosterol. The values of percentage RSD for intraday and interday precision were found to be within the accepted limits for analytical methods (<15%). Selectivity, linearity, LOD, LOQ, accuracy, and precision were evaluated for all three phytoconstituents as per International Conference on Harmonization guidelines. Conclusions The proposed method is accurate and sensitive and can be used for the routine quantification of betulinic acid, lupeol, and β-sitosterol from the herbal extract and its poly-herbal formulations.
Preetiben N. Yadav, Usmangani K. Chhalotiya, Heta M. Kachhiya, Keshaben M. Patel, and Dimal A. Shah
Informa UK Limited
Abstract A sensitive, selective, accurate, precise and robust thin layer chromatographic method has been developed and validated for the estimation of β-Adrenergic Receptor agonist drug Mirabegron in bulk and pharmaceutical formulation. Aluminium supported plates pre-coated with silica gel 60F-254 was used as stationary phase while methanol: acetonitrile: triethylamine (4: 6: 0.1, v/v/v) mixture saturated in twin trough chamber was used as mobile phase. The Rf values of Mirabegron was observed to be 0.58 ± 0.0089. The detection was carried out in absorbance mode at 247 nm. Linear regression analysis data showed linear relationship for Mirabegron over a concentration range of 100-1200 ng/band. Forced degradation study showed drug was susceptible to acid and alkali hydrolysis, chemical oxidation and photo degradation. The degraded product peaks of Mirabegron were well resolved from the parent peak as data obtained from their significant Rf values. The method was validated and data from forced degradation study showed that the method can be used for quantifying Mirabegron in marketed formulation.
P. Jay, Jinal N. Tandel, Usmagani Chhalotiya and Kirtan Patel
A strategic specific and sensitive quantitative analysis of Minoxidil and Finasteride has been developed by using HPLC with reliable, precise, and accurate result in bulk and marketed formulation. In this method Phenomenex C 18 (250 mm × 4.6 mm, 5 μm) column was used as stationary phase and a composition of Methanol: Water (85:15 v/v) was used as mobile phase. An isocratic elution programming has been done at a flow rate of 1 mL min -1 . The eluted analytes show appreciable absorbance at 223 nm. The proposed RP-LC method was validated according to ICH guidelines. The retention time of Minoxidil and Finasteride was found to be 3.15 min and 4.36 min respectively. The method was found to be linear over a range of 6 – 54 µg mL -1 for Minoxidil and 0.2-1.8 µg mL -1 for Finasteride. The percentage recovery was found to be 99.88-100.85 % for Minoxidil and 99.99-100.33 % for Finasteride. The proposed reverse phase LC method has potential qualitative as well as quantitative applications for simultaneous estimation of Minoxidil and Finasteride in bulk and pharmaceutical dosage form.
Kirtan Patel, Usmangani Chhalotiya, Hetaben Kachhiya, Jay Patel, Dimal Shah, and Dhruti Nagda
Wiley
Devansh A. Kansara, Usmangani K. Chhalotiya, Heta M. Kachhiya, Ishita M. Patel, and Dimal A. Shah
Springer Science and Business Media LLC
Ishita M. Patel, Usmangani K. Chhalotiya, Harsha D. Jani, Devansh Kansara, and Dimal A Shah
Springer Science and Business Media LLC
Devansh Kansara, Usmangani K. Chhalotiya, Hetaben M. Kachhiya, and Ishita Patel
ACG Publications
An accurate, sensitive, robust and precise high performance thin layer liquid chromatography method was developed based on ICH Q2 (R1) guidelines for estimation of novel combination of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium in bulk and its synthetic mixture. Pre-coated silica gel aluminum plate 60 F254 was selected as the stationary phase and n-hexane, n-butanol, methanol, and Glacial Acetic Acid (5.7:2:2.3:0.1, v/v/v/v) was selected as mobile phase. All three drugs showing appreciable absorbance at the common wavelength of 242 nm were selected for quantification of Amlodipine besylate, Rosuvastatin calcium, and Fimasartan potassium, respectively. The method was validated for linearity, precision, accuracy, and robustness, limit of detection and limit of quantitation as per ICH parameters. The regression coefficients (r2) were found to be 0.9986, 0.9975 and 0.9988 for Amlodipine besylate, Rosuvastatin calcium, and Fimasartan potassium, respectively. The average percentage recovery of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium were found to be 99.38-100-60%, 99.75-100.63%, 99.39-100%, respectively. Thin Layer Chromatographic method has prospective qualitative as well as quantitative applications for concurrent estimation of Amlodipine besylate, Rosuvastatin calcium and Fimasartan potassium in bulk and pharmaceutical dosage form.
Dimal Shah, Ishita Gondalia, Vandana Patel, Ashok Mahajan, and Usmangani K. Chhalotiya
ACG Publications
Accurate and precise reverse phase liquid chromatographic method has been developed for the estimation Remogliflozin etabonate in bulk and tablet dosage form. Reverse phase C18 column was used as stationary phase along with mixture of methanol:water (70:30%, v/v) as a mobile phase. Mobile phase flow rate was maintained at 1mL/min and analysis was performed at 229 nm. The method was linear in the concentration range of 1 – 25 μg/mL with correlation coefficient (r) 0.997. The proposed method was validated with respect to linearity, accuracy, precision and robustness as per ICH Q2 (R1) guideline. To find out the possible degradation pathway, forced degradation studies were performed. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time value. The drug was found to be highly susceptible to acid and base hydrolysis. The developed method can be used for analysis of stability samples and routing quality control evaluation of Remogliflozin etabonate in tablet formulation.
Anjali M Thakkar, Usmangani K Chhalotiya, Nikunj Parekh, Jaineel V Desai, and Dimal A Shah
Oxford University Press (OUP)
Abstract A sensitive, selective and precise high performance thin layer chromatographic method has been developed and validated for the quantification of Brexpiprazole in bulk drug and in pharmaceutical dosage form. The method employed HPTLC aluminum plates (pre-coated with silica gel 60 F254) as stationary phase while n-butanol was used as mobile phase. The Rf value of Brexpiprazole was observed to be 0.38. The densitometric analysis was carried out in absorbance mode at 215 nm. The linear regression analysis data for the calibration plots showed a good linear relationship for Brexpiprazole over a concentration range of 200–1,600 ng band−1. The limit of detection and limit of quantification for Brexpiprazole was found to be 66 and 200 ng band−1. To find out the possible degradation pathway, forced degradation studies were performed. The stock solutions of Brexpiprazole (1,000 μg mL−1) were subjected to acid and alkali hydrolysis, chemical oxidation, dry heat degradation and photo degradation. The drug was found to be susceptible to acid and alkali hydrolysis, chemical oxidation, photo degradation and dry heat. The degraded product peaks were well resolved from the pure drug peak with significant difference in their Rf values. Stressed samples were analyzed using developed HPTLC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of Brexpiprazole in marketed formulation and determination of content uniformity of tablet formulation. Statistical analysis showed that the method is repeatable, selective, and precise.
Dimal A. Shah, Jaimin S. Patel, Priyanka Jadeja, Vandana B. Patel, and Usmangani K. Chhalotiya
Informa UK Limited
ABSTRACT A precise and accurate method for the analysis of antihypertensive drug combination nifedipine and valsartan was developed using the HPTLC method. The stationary phase used was a pre-coated silica gel G60 – F254 aluminium sheet and the mobile phase was acetonitrile: methanol: n-butanol: acetic acid (6:2:2:0.1, v/v/v/v). The detection of spots was carried out densitometrically using a UV detector at 230 nm in the absorbance mode. The Rf values of valsartan and nifedipine were found to be 0.25 and 0.65, respectively. The calibration curve was found to be linear in the range of 120–320 ng/band and 900–2400 ng/band for nifedipine and valsartan, respectively. Forced degradation studies were performed using stress conditions like acid and base hydrolysis, photolytic, thermal and oxidative stress degradation to develop the stability indicating method. The degradation study indicated that nifedipine was susceptible to acid-base hydrolysis, oxidative stress degradation and photolytic degradation, while valsartan was susceptible to acid-base hydrolysis and oxidative stress degradation.
Dimal A. Shah, Pooja J. Tahilramani, Vandana B. Patel, and Usmangani Chhalotiya
Akademiai Kiado Zrt.
A sensitive and precise high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous estimation of mirabegron and solifenacin succinate in combination. The method employed HPTLC aluminum plates pre-coated with silica gel 60 F254 as the stationary phase and methanol—ethyl acetate—triethylamine (8:2:0.1, V/V) as the mobile phase. The RF value was observed to be 0.76 and 0.56 for mirabegron and solifenacin succinate, respectively. Densitometric analysis was carried out in the absorbance mode at 222 nm. The method was linear in the range of 2–5.5 µg per band for mirabegron and 0.4–1.1 µg per band for solifenacin succinate. The method was validated as per the International Conference on Harmonisation (ICH) guideline and applied successfully for the estimation of both drugs in a physical mixture.
Dharmendra Jayantibhai Prajapati, Usmangani Khalilurraheman Chhalotiya, Minesh Dahyabhai Prajapati, Jalpa Upendrabhai Patel, and Jaineel Vinodrai Desai
Bentham Science Publishers Ltd.
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;
Vandana B. Patel, Dimal A. Shah, Hemaxi B. Gohil, and Usmangani Chhalotiya
Akademiai Kiado Zrt.
A sensitive and precise high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous estimation of clozapine and aripiprazole in combination. The method employed HPTLC aluminum plates pre-coated with silica gel 60 F254 as the stationary phase, while the solvent system was toluene–methanol–ethyl acetate–ammonia (6.5:2.5:1:0.1, v/v). The RF values were observed to be 0.43 and 0.60 for clozapine and aripiprazole, respectively. Densitometric analysis was carried out in absorbance mode at 218 nm. The method was linear in the range of 200–1600 ng per band for clozapine and 100–800 ng per band for aripiprazole. The stress degradation study was performed, and it was found that clozapine was susceptible to acid hydrolysis, base hydrolysis, and photolytic degradation study. Aripiprazole was susceptible to oxidative stress degradation study. The method was validated and applied successfully for the estimation of both drugs in the synthetic mixture.
Brijesh Patel, Usmangani K. Chhalotiya, and Sandip B. Patel
SciELO Agencia Nacional de Investigacion y Desarrollo (ANID)
A sensitive, accurate, precise and reproducible high performance thin layer chromatographic method has been developed for the estimation of clofarabine in their pharmaceutical dosage form. The objective of this validation of an analytical procedure is to demonstrate that the drug Clofarabine is suitable for its intended purpose. The analytical method development recommends the quality, purity and specificity of the drug. Clofarabine injection form during the manufacturing process and hence the standard of drug may not vary, which produce the desirable therapeutic effect.TLC aluminum plates pre-coated with silica gel 60F 254 used as the stationary phase, while toluene: methanol (8:2, v/v) used as mobile phase. The Rf value was observe 0.34± 0.05 for clofarabine. The densitometric analysis was carried out in absorbance mode at 266 nm. The method was linear in the range of 50 – 1000 ng/spot for clofarabine. The method was validated as per ICH guideline. The limit of detection and limit of quantitation were found to be 17.60ng/spot and 53.35 ng/spot, respectively for clofarabine.The proposed method was successfully applied to the estimation of clofarabinein the pharmaceutical dosage form. Clofarabine was subjected to acid and alkali hydrolysis, chemical oxidation, wet hydrolysis, dry heat degradation and sun light degradation. The degradants peaks were well resolved from the pure drug peak with significant difference in their R f values. Stressed samples were assayed using proposed TLC method.
Jalpa U. PATEL, Usmangani K. CHHALOTIYA, and Purvi A. SHAH
Galenos Yayinevi
Objectives: First derivative synchronous spectrofluorimetry has been found to be superior because of its highly specific spectral discrimination and readily available solvent, it is economical, eco-friendly, and lacks an extraction procedure. Materials and Methods: In the present study, a new simple, sensitive, and time-saving first derivative synchronous spectrofluorimetry method has been developed for simultaneous estimation of clonazepam (CLO) and paroxetine hydrochloride (PH) in pharmaceutical dose forms. Results: CLO was determined at the emission wavelength of 512.79 nm (zero-crossing wavelength point of PH). Similarly, PH was measured at 336.00 nm (zero-crossing wavelength point of CLO). The first derivative amplitude-concentration plots were rectilinear over the range of 1-5 μg/ mL for CLO and 5-25 μg/mL for PH. The method was validated statistically as per the ICH guidelines. The limits of detection were 0.055 and 0.033 μg/mL and quantification limits were 0.169 and 0.102 μg/mL for CLO and PH, respectively. The percentage recovery in commercial formulation was found to be in the range 100.45% and 99.38% for CLO and PH, respectively, by the proposed method, and percent relative standard deviation values for precision and accuracy studies were found to be less than 2. Conclusion: This spectrofluorimetry method has been found to have several advantages such as simple spectra, high selectivity, and low interference. By virtue of its high sensitivity, this method could be applied to the analysis of both CLO and PH in their co-formulated dose forms.