Analysis Of Pharmaceutical Dosage Forms Research Articles

Coupling of physical extraction and mathematical filtration in spectrophotometric analysis of natural therapy essential for prophylaxis and treatment of COVID-19 infection - Comparative study along with greenness evaluation

Diosmin (DIO) and hesperidin (HSP) are important classes of flavonoid glycoside effectively used to prevent comorbid diseases that are commonly associated with COVID-19. An innovative, green, ccurate, effective, cost, and timeless spectrophotometric strategy was established to analyze such challengeable mixture in a co-formulated tablet namely Diosed C® tablets that comprises DIO, HSP and vitamin C (VIT. C) in the ratio of (450 mg: 50 mg: 100 mg) necessary for prevention and treatment of COVID-19. Vitamin C was resolved through physical extraction using de-ionized water while DIO and HSP were extracted via spectrophotometric methods using two different solvents [0.1 M NaOH or solvent blend consisting of DMSO and methanol (1:1)]. Mathematical filtration technique is successfully applied to recover the parent spectra of both DIO and HSP via three methods which are absorbance resolution (AR), Induced absorbance resolution (IAR) and ratio extraction (RE). VIT. C was successfully analyzed in de-ionized water using its maxima at 266.0 nm in a linearity range 2.0–20.0 μg/mL, DIO was effectively determined in 0.1 M NaOH at 372.0 nm in a linearity range of 7.0–70.0 μg/mL as well as in solvent blend at 344.0 nm in linearity range of 5.0–55.0 μg/mL while HSP was accurately analyzed in 0.1 M NaOH at 240.0 nm in linearity range of 3.5–50.0 μg/mL as well as in solvent blend at 285.0 nm in linearity range of 4.0–50.0 μg/mL. Satisfactory results were accomplished when conducting ICH guidelines for assuring the methods validation. Comparative study was introduced in the analysis of such critical combination and was prosperously devoted for the effective analysis of pharmaceutical dosage form. The proposed extraction pathways undergo the guidelines of green analytical chemistry using Analytical Eco-Scale (AES), AGREE and GAPI greenness assessment tools which confirmed their eco-friendly nature with priority to 0.1 M NaOH. The obtained results of the suggested methods were set side by side with those of official/reported methods statistically and show satisfactory implications. The presented methods were simple, affordable, smoothly applicable and their results were acceptable that enhances their usage and application in the quality control laboratories.

Dissolution Method development and validation for simultaneous determination of Metformin and Teneligliptin in pharmaceutical tablets

We have developed and validated an inexpensive, selective, simple, and precise HPLC-RP dissolution method for estimating the concentration of Metformin and Teneligliptin in combination dosage form. This experimental analysis was performed on a reverse phase high performance high-performance liquid chromatography, (RP-HPLC) column (250mm x 4.6mm, 5µm) by using Mobile phase Acetonitrile and Potassium Dihydrogen Phosphate with concentration 0.05 M and buffer with pH-7.0 at a flow rate of 1.0ml/min and the detected at wavelength 225nm. In line with ICH guidelines, the linearity of the analytical method was discovered to be in the range of 7.0 to 21.00g/ml for Metformin. The linearity of the method for Teneligliptin was 22.5-67.5g/ml. Metformin and Teneligliptin had correlation coefficients greater than 0.990. The relative standard deviation value for system precision and method was less than 2.0%. All statistical data proves validity of the method and can be used for routine analysis of pharmaceutical dosage form.

ARP-HPLC STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF NETUPITANT AND PALONOSETRON IN PHARMACEUTICAL DOSAGE FORM

Objective: A simple, precise, sensitive, rapid, accurate, and specific method was developed and validated for the simultaneous determination of Netupitant and Palonosetron in Pharmaceutical dosage form. Methods: The separation was done on the ODS C18 column of dimensions (150 mm x 4.6, 5 μm) with the mobile phase 0.1N potassium dihydrogen orthophosphate pH 3.3 and acetonitrile in a 50:50 ratio, at a flow rate of 1.0 ml/min and injection volume of 10 μl. The optimum wavelength selected was 274 nm and the temperature of the column was maintained at 30 ℃. Results: The retention time was 2.199 min and 2.893 min and they were linear in the concentration range of 75-450 μg/ml and 0.125-0.75 μg/ml for Netupitant and Palonosetron, respectively. The repeatability and intermediate precision were found to be within acceptable limits. Regression equation of Netupitant and Palonosetron is Y=6329x+42914 and Y= 258884x+3103.9, respectively. LOD was found to be 0.33μg/ml, 0.99μg/ml and LOQ was 0.01μg/ml, 0.04μg/ml for Netupitant and Palonosetron. The correlation coefficient (R2) value was found to be 0.999 and %recovery was obtained as 100.32%and 99.6% for Netupitant and Palonosetron, respectively. Forced degradation studies reveal that the drugs are unstable under acidic conditions. Conclusion: The flexibility, accuracy, precision of the developed method ensures applicability in routine analysis of pharmaceutical dosage form.

New UPLC method development and validation for simultaneous estimation of netiputant and palonosetron using bulk and pharmaceutical dosage form using UPLC

A simple and selective LC method is described for the determination of Netupitant and Palonosetron in tablet dosage forms. Chromatographic separation was achieved on a Inertsil ODS (C18) RP Column (250mm x 4.6 mm. 5µm) column using mobile phase consisting of a 55 volumes of mixed phosphate buffer and 45 volumes of acetonitrile were prepared with detection of 253nm. Linearity was observed in the range 25-125 µg/ml for Netupitant (r 2 =0.995) and 50-150 µg /ml for Palonosetron (r 2 =0.999) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.

A Novel UPLC Method for Simultaneous Estimation of Ertugliflozin and Sitagliptin in Bulk and Tablet Dosage Form

Aim: The proposed study aimed to develop a novel ultra-performance liquid chromatography (UPLC) method for the estimation of Ertugliflozin and Sitagliptin in Bulk and Tablet dosage form and validate the method in accordance with the International Conference on Harmonization guidelines. Methods: The optimized conditions for the developed UPLC method are Acquity UPLC HIBRA C18 (100mm × 2.1mm, 1.8µ) column maintained at 30°C with a mobile phase consisting of Buffer (0.01N sodium hydrogen phosphate) pH adjusted to 4.0 with dil. orthophosphoric acid: Acetonitrile in the ratio of 60:40%v/v on isocratic mode at a flow rate of 0.3mL/min. Results and conclusion: The sample was detected at 220nm. The retention time for Ertugliflozin and Sitagliptin was deemed at 1.873min and 1.260min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness, and solution stability. The method obeyed Beer’s law in the concentration range of 3.75µg/mL to 22.5µg/mL for Ertugliflozin and 25µg/mL to 150µg/mL for Sitagliptin with a correlation coefficient of 0.999 for Ertugliflozin and Sitagliptin respectively. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that the drug is stable in stressed conditions. The developed method for the estimation of Ertugliflozin and Sitagliptin can be utilized for the routine analysis of Pharmaceutical dosage form.

Simultaneous Determination of Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin in Bulk Drug and Formulation by UPLC Q-TOF-MS

Background: A simple and sensitive Ultra Performance Liquid Chromatography-Mass Spectrometry method was developed and validated to measure the concentrations of Alogliptin (ALO), Linagliptin (LIN), Saxagliptin (SAX), and Sitagliptin (SIT) using Pioglitazone (PIO) as an internal standard. Methods: Chromatographic separation of six gliptins was achieved on a C-18 column (100×2.1 mm, 2.7 μm) using a mobile phase consisting of formic acid in water, 0.1%v/v: acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. Targeted MS/MS mode on a QTOF MS was used to quantify the drug utilizing the transitions of 340.1(m/z), 473.2 (m/z), 316.2 (m/z), 408.1 (m/z), and 357.1 (m/z) for ALO, LIN, SAX, SIT and PIO respectively. Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear over the concentration ranges of 1516.0-4548.1 ng mL-1, 519.8- 1559.4 ng mL-1, 1531.4-4594.3 ng mL-1and 1519.6-4558.8 ng mL-1 for ALO, LIN, SAX and SIT respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8 _ 0.76 % (GEM), 102.2 _ 1.59 % (LIN), 95.3 _ 2.74 % (SAX) and 99.2 _ 1.75 % (SIT) respectively. Conclusions: The optimized validated UPLC QTOF-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity. The optimized method is suitable for application in quantitative analysis of pharmaceutical dosage forms for QC laboratory.

Method development and validation of aspirin and clopidogrel pharmaceutical dosage forms by developing new RP HPLC method

A simple and selective LC method is described for the determination of Aspirin and Clopidogrel in tablet dosage forms. Chromatographic separation was achieved on a c18 column along with mobile phase consisting of a combination of fifty five volumes of Mixed Phosphate Buffer and forty five volumes of Acetonitrile with detection of 235 nm. Linearity was observed in the range 20-60 μg/ml for Aspirin (r2=0.998) and 10-30 μg /ml for Clopidogrel (r2 =0.998) for the amount of drugs estimated by the projected ways was in smart agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD trials. All statistical data proves validity of the ways and may be used for routine analysis of pharmaceutical dosage form.

STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF PANOBINOSTAT LACTATEIN PHARMACEUTICAL DOSAGE FORMS BY UPLC

Objective: The present study aimed to develop a stability indicating ultra-performance liquid chromatography (UPLC) method for the estimation of panobinostat lactate in pharmaceutical dosage form and validate the method in accordance with ICH guidelines.Methods: The optimized conditions for the developed UPLC method are acquity UPLC hibar C18 (100 mm × 2.1 mm, 1.8µ) column maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 50:50%v/v on isocratic mode at flow rate 0.3 ml/min. The sample was detected at 266 nm.Results: The retention time for panobinostat was found to be 1.6 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability. The method obeyed Beer’s law in the concentration range of 50µg/ml and 300µg/ml with correlation coefficient of 0.9998. Forced degradation studies were conducted by exposing the drug solution to various stress conditions such as acidic, basic, peroxide, neutral, photolytic and thermal conditions. The net degradation was found to be within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation ofpanobinostat can be utilized for the routine analysis of pharmaceutical dosage form.

STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF CABOZANTINIB IN PHARMACEUTICAL DOSAGE FORMS BY ULTRA-PERFORMANCE LIQUID CHROMATOGRAPHY

Objective: The proposed study aimed to develop a stability-indicating ultra-performance liquid chromatography (UPLC) method for the estimation of cabozantinib in pharmaceutical dosage form and validate the method in accordance with the International Conference on Harmonization guidelines.Methods: The optimized conditions for the developed UPLC method are Acquity UPLC Hibar C18 (100 mm × 2.1 mm, 1.7 μ) column maintained at 30°C with mobile phase consisting of 0.1% orthophosphoric acid and acetonitrile in the ratio of 55:45% v/v on isocratic mode at flow rate of 0.3 mL/ min. The sample was detected at 244 nm.Results: The retention time for cabozantinib was deemed 1.3 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness, and solution stability. The method obeyed Beer’s law in the concentration range of 20 μg/mL and 120 μg/mL with correlation coefficient of 0.9997. Forced degradation studies were conducted by exposing the drug solution to numerous stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was considered within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation of cabozantinib can be utilized for the routine analysis of pharmaceutical dosage form.

NEW STABILITY-INDICATING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF LENVATINIB MESYLATE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORMS

Objective: The objective of the present study was to develop and validate a new stability-indicating method for the quantification of lenvatinib mesylate in bulk drug and pharmaceutical dosage form using ultra performance liquid chromatography (UPLC).Methods: The optimized chromatographic conditions for elution of drug included UPLC HSS C18 (100 mm × 2.1 mm, 1.8 m) column, mixture of 0.1% orthophosphoric acid and acetonitrile (50:50 v/v%) mobile phase run on an isocratic mode at a flow rate of 0.3 mL/min, 240 nm detection wavelength, and column oven temperature maintained at 30°C.Results: The retention time for lenvatinib was found to be 1.24 min. The developed method was validated for various validation parameters in accordance with the International Conference on Harmonization guidelines. The method obeyed Beer’s law in the concentration range of 2.5– 15 μg/mL with a correlation coefficient of 0.9996. The percentage relative standard deviation and percentage recovery were determined to be 0.4 and 99.66–100.30%, respectively. The developed method was found to be accurate, precise, specific, linear, rugged, and robust. Forced degradation studies were conducted by exposing the drug to diverse stress conditions such as acidic, basic, peroxide, neutral, photolytic, and thermal conditions. The net degradation was obtained within the limits.Conclusion: The developed method for the estimation of lenvatinib can be employed to routine analysis of pharmaceutical dosage form.

SPECTROPHOTOMETRIC DETERMINATION OF PROPRANOLOL HYDROCHLORIDE AND METOPROLOL TARTRATE IN PHARMACEUTICAL DOSAGE FORMS, SPIKED WATER AND BIOLOGICAL FLUIDS

Objective: A new spectrophotometric method for the determination of propranolol hydrochloride (PRO) and metoprolol tartrate (MTP), beta blocker drugs, has been developed for their analysis in pharmaceutical dosage forms for the purpose of quality control and water samples for monitoring impact on environmental water quality of natural sources and in biological fluids for ascertaining their physiological performance.Methods: The method is based on the derivatization of the amino function present in these drugs to the corresponding yellow copper (I) drug dithiocarbamate derivative through reaction with carbon disulphide, pyridine and copper (I) perchlorate in aqueous acetonitrile and measuring absorbance at 406 nm for propranolol and 400 nm for metoprolol. The different experimental parameters affecting the development and stability of the colour were carefully studied and optimized.Results: The Beer’s law is obeyed in the range of 1.0-40.0 μg/ml of each drug solution with a correlation coefficient 0.999. The maximum relative standard deviations (RSDs) in the analysis of pure PRO and MTP were 1.01 and 1.52 % respectively. The recoveries of the drugs from pharmaceutical formulations, spiked water samples and biological fluids were in the range 98.0-100.5 % with RSDs in the range 0.23-1.94% indicating good accuracy and precision of the method.Conclusion: The instantaneous development of colour and its stability, well-established stoichiometry of the reaction and above simplicity and rapidity of procedures are some special attributes of the proposed method.

Sensitive Voltammetric Detection of Metronidazole Based on Three-Dimensional Graphene-Like Carbon Architecture/Polythionine Modified Glassy Carbon Electrode

An ultrasensitive electrochemical sensing platform based on three-dimensional (3D) graphene-like carbon architecture (3D-HPG) and polythionine (PTH) modified glassy carbon electrode (GCE) was developed for the determination of metronidazole. The 3D-HPG/PTH interface possesses 3D porous structure, large electro-active surface area and excellent electrical conductivity. Electrochemical behavior of metronidazole at the 3D-HPG/PTH/GCE was investigated by cyclic voltammetry (CV), and it has been found that the 3D-HPG/PTH nanocomposite exhibited synergistic electro-catalytic property for the reduction of metronidazole. Under the optimized conditions, metronidazole was determined by CV and differential pulse voltammetry (DPV). DPV was found to be more effective for detecting low concentrations of metronidazole. Two linear ranges of 0.05−70 μM and 70−500 μM were obtained, with a detection limit of 1 nM (S/N = 3). The 3D-HPG/PTH/GCE exhibits high sensitivity, good selectivity, satisfactory reusability and reproducibility. It was applied for the determination of metronidazole in real water samples, with satisfactory recoveries ranging from 92.8% to 103%, and was successfully applied for the analysis of pharmaceutical dosage form.

Development and methodology for the estimation of bisaprolol in pharmaceuticals

Introduction. The number of drugs introduced into the pharmaceutical market is increasing every year. These drugs may be either new entities or partial structural modification of the existing one. The objective of any analytical measurement is to obtain consistent, reliable and accurate data. Thin layer chromatography, or TLC, is a method for analyzing mixtures by separating the compounds in the mixture. TLC can be used to help determine the number of components in a mixture, the identity of compounds, and the purity of a compound.Aim: Analysis of bisoprolol is described in Pharmacopeia but aim of our researches was to improve to more simple, selective, more accurate, precise, reliable, less expensive methods by TLC of bisoprolol in pharmaceuticals and for using this methods for analysis of their metabolites in next step of researches. Materials and Methods: The present study is assessed system solvents of bisoprolol for thin layer chromatography.Results and Discussion: Method of identification of bisoprolol in medicines by TLC has been developed. Established that the most optimal Rf observed using mobile phases: ammonia (25%)-propanol (30: 70). The detection limits of bisoprolol in this system is 0.4 mcg. We explored the validation characteristics - specificity and suitability of the chromatographic system that met, the eligibility criteria established by the SPU.Conclusion: We have been developed chromatographic method of identification of bisoprolol in pharmaceuticals. The proposed method is economical, simple and applicable to the analysis of pharmaceutical dosage forms.

DEVELOPMENT OF METHODS FOR IDENTIFICATION OF CALCIUM CHANNEL BLOCKERS IN MEDICINES

The pharmaceutical analysis has got more emphasis to satisfy our query for better understanding of physico - chemical properties of pharmaceutical compounds, by the use of advanced instrumen tal methods . Calcium channel blockers are used as antihypertensive drugs, i . e . , as medications to decrease blood pressure in patients with hypertension . Analysises of amlodipine, v erapamil, nifedipine are described in Pharmacopeia but aim of our researches was to improve to more rapid, simple, selective, more accurate, precise, reliable, less expensive methods by TLC of amlodipine, verapamil, nifedipine in medicines and for using this methods for analysis of their metabolites in next step of researches . Met hods of identifi cation of amlodipine, nifedipine and verapamil in medicines by TLC have been developed . Established that the most optimal Rf observed using mobile phases : propanol R - water R ( 7 0 : 30 ) for amlodipine and chloroform R - propanol R ( 9 : 1 ) for ni fedipine and n - butanol - methanol ( 3 : 2 ) for verapamil . The detection limit s of amlodipine, nifedipine and verapamil in these systems are 0 . 4 m c g . However, those mobile phases are the most express . W e explored the validation characteristics - specificity and suitability of the chromatographic system that met , the eligibility criteria established by the SPU . In conclusion, we have been d eveloped chromatographic methods of identification and quantification of amlodipine, verapamil, nifedipine in medicines . The p roposed methods are rapid, economical, simple, accurate, selective, precise and applicable to the analysis of pharmaceutical dosage forms . These methods can also give excellent results and can be employed for the routine analysis .

Resolution of overlapped spectra for the determination of ternary mixture using different and modified spectrophotometric methods

Four new spectrophotometric methods were developed, applied to resolve the overlapped spectra of a ternary mixture of [aliskiren hemifumarate (ALS)–amlodipine besylate (AM)–hydrochlorothiazide (HCT)] and to determine the three drugs in pure form and in combined dosage form. Method A depends on simultaneous determination of ALS, AM and HCT using principal component regression and partial least squares chemometric methods. In Method B, a modified isosbestic spectrophotometric method was applied for the determination of the total concentration of ALS and HCT by measuring the absorbance at 274.5nm (isosbestic point, Aiso). On the other hand, the concentration of HCT in ternary mixture with ALS and AM could be calculated without interference using first derivative spectrophotometric method by measuring the amplitude at 279nm (zero crossing of ALS and zero value of AM). Thus, the content of ALS was calculated by subtraction. Method C, double divisor first derivative ratio spectrophotometry (double divisor 1DD method), was based on that for the determination of one drug, the ratio spectra were obtained by dividing the absorption spectra of its different concentrations by the sum of the absorption spectra of the other two drugs as a double divisor. The first derivative of the obtained ratio spectra were then recorded using the appropriate smoothing factor. The amplitudes at 291nm, 380nm and 274.5nm were selected for the determination of ALS, AM and HCT in their ternary mixture, respectively. Method D was based on mean centering of ratio spectra. The mean centered values at 287, 295.5 and 269nm were recorded and used for the determination of ALS, AM and HCT, respectively. The developed methods were validated according to ICH guidelines and proved to be accurate, precise and selective. Satisfactory results were obtained by applying the proposed methods to the analysis of pharmaceutical dosage form.

Bio-analytical method development and validation for the estimation of Clotrimazole in human plasma by RP-HPLC method

The present study Estimation of drugs in biological media is increasingly important nowadays, which reveals information like bioavailability, bioequivalence, drug abuse, and pharmacokinetics and drug research. HPLC is the most suitable technique for the analysis of biological fluids owing to its well-developed characteristics and ruggedness. It is an extremely sensitive, precise, accurate, and rapid, separation technique. Clotrimazole is a broad spectrum antifungal agent that is used for the treatment of infections caused by various species of pathogenic dermatophytes, yeasts, and Malassezia furfur. The primary action of Clotrimazole is against dividing and growing organisms. Clotrimazole interacts with yeast 14-α demethylase, a cytochrome P-450 enzyme that converts lanosterol to ergosterol, an essential component of the membrane. In this way, Clotrimazole inhibits ergosterol synthesis, resulting in increased cellular permeability. Few analytical methods were reported for the quantitative determination of Clotrimazole and its combination with other drugs by HPLC. Only one method was reported for Clotrimazole in mice plasma by capillary electrophoresis. But there is no RP-HPLC method reported for the bio-analytical method development in human plasma using protein precipitation method under different chromatographic conditions. The present study is planned to develop newer analytical method for the determination of Clotrimazole by bio-analytical method development in human plasma using protein precipitation by RP-HPLC under different chromatographic conditions. CONCLUSION: A bioanalytical method was developed for the estimation of Clotrimazole by HPLC method. The method was validated for its transferability to other user or other laboratory. The HPLC method was developed by using 0.5%TEA in water (pH 3 adjusted with Orthophosphoric acid) and Acetonitrile in meticulous ratio. The peaks obtained for the drugs of interest by the present method are well resolved from each other without any interference and from the plasma endogenous proteins. The peaks are symmetrical with acceptable tailing factor. The retention time of Clotrimazole was within the limit. The results of linearity, intraday and interday precision study and capability of the extraction method were within the limits of bioanalytical method development. The method was linear with a correlation coefficient of acceptable agreement, which is suitable for the estimation of Clotrimazole in human plasma and other biological fluids. The method demonstrated relative recoveries with acceptable relative standard deviation. The limit of quantification (LOQ) and limit of detection (LOD) for Clotrimazole was found to be nanograms lesser than unity. Hence the developed method is sensitive for the estimation of Clotrimazole in trace amounts. Peak purity studies, with peak purity index values closer to unity reveals that the method developed was specific for the estimation of Clotrimazole in blood and other biological fluids. It can be concluded that the developed RP-HPLC method in human plasma was found to be very simple, reliable and selective for providing satisfactory accuracy and precision. The methods are suitable for routine quantitative analysis in pharmaceutical dosage forms. Hence this developed method can be used further in Bioequivalence and bioavailability studies of clotrimazole. Pharmacokinetic and bio-equivalence study centers

A novel electroanalytical nanosensor based on MWCNT/Fe2O3 nanoparticles for the determination of antiparkinson drug ropinirole

A carbon paste electrode modified by –COOH functionalized multiwalled carbon nanotubes and Fe2O3 nanoparticles was prepared for the determination of antiparkinson drug ropinirole using adsorptive stripping differential pulse and square wave voltammetric methods. The results showed that the modified electrode significantly enhanced the oxidation peak current of ropinirole. Effects of pH, scan rate, and electrolyte type on the determination of ropinirole were analyzed. Ropinirole gave two irreversible anodic peaks at modified electrode in pH 6.0 phosphate buffer solution; studies were realized for the peak which was more positive potential (peak 2). Limit of detection values were 1.30 × 10−3 μg mL−1 and 4.08 × 10−4 μg mL−1 for peak 2 with adsorptive stripping differential pulse and square wave voltammetric methods, respectively. The proposed methods were applied to analysis of pharmaceutical dosage form containing ropinirole. The recovery studies with values of 105.50 and 100.88 % showed the accuracy of these methods. The number of transferred electrons was investigated.

Simultaneous determination of linagliptin and metformin by reverse phase-high performance liquid chromatography method: An application in quantitative analysis of pharmaceutical dosage forms.

To enhance patient compliance toward treatment in diseases like diabetes, usually a combination of drugs is prescribed. Therefore, an anti-diabetic fixed-dose combination of 2.5 mg of linagliptin 500 mg of metformin was taken for simultaneous estimation of both the drugs by reverse phase-high performance liquid chromatography (RP-HPLC) method. The present study aimed to develop a simple and sensitive RP-HPLC method for the simultaneous determination of linagliptin and metformin in pharmaceutical dosage forms. The chromatographic separation was designed and evaluated by using linagliptin and metformin working standard and sample solutions in the linearity range. Chromatographic separation was performed on a C18 column using a mobile phase of 70:30 (v/v) mixture of methanol and 0.05 M potassium dihydrogen orthophosphate (pH adjusted to 4.6 with orthophosphoric acid) delivered at a flow rate of 0.6 mL/min and UV detection at 267 nm. Linagliptin and metformin shown linearity in the range of 2-12 μg/mL and 400–2400 μg/mL respectively with correlation co-efficient of 0.9996 and 0.9989. The resultant findings analyzed for standard deviation (SD) and relative standard deviation to validate the developed method. The retention time of linagliptin and metformin was found to be 6.3 and 4.6 min and separation was complete in <10 min. The method was validated for linearity, accuracy and precision were found to be acceptable over the linearity range of the linagliptin and metformin. The method was found suitable for the routine quantitative analysis of linagliptin and metformin in pharmaceutical dosage forms.

Determination of pseudoephedrine, paracetamole and ascorbic acid in multicomponent powder using reversed-phase chromatographic method

For the simultaneous analysis of multicomponent mixture containing pseudoephedrine, paracetamole and ascorbic acid two RP-HPLC methods were developed. Separation were performed on Hewlett Packard 1100 system which consisted of HP 1100 binary pump, HP 1100 UV/VIS detector and HP ChemStation for the automatic data evaluation. Methods were developed, e. g. chromatographic conditiond settled, methods submited to method validation and then applied for the determination of content of multicomponent powder.The best separation was achived on Platinium Alltech Amino 150 x 4.6 mm, 5 mm particle size column, at 30°C. Injection volume was 20mL. Mobile phase in mehtod I was a mixture of methanol-water (30:70 V/V), pH 2.5, and in mehtod II was a mixture methanol-water (60:40 V/V), pH 2.9. pH of the mobile phases were adjusted with 85% ortophosphoric acid. Detection was performed at 214 nm in mehtod I and at 257 nm in method II. Flow rate was 1 mLmin-1. Developed methods were validated. Obtained results showed that both methods are suitable for routine analysis of pharmaceutical dosage forms which contain pseudoephedrine, paracetamole and ascorbic acid.

A Sensitive and Selective RP-LC Method for the Simultaneous Determination of the Antihypertensive Drugs, Enalapril, Lercanidipine, Nitrendipine and Their Validation

A RP-LC method is presented, which is sensitive and selective for the simultaneous determination of enalapril–lercanidipine and enalapril–nitrendipine binary mixtures in their pharmaceutical dosage forms. The analyte peaks were detected using the LC method with the mobile phase ratio of methanol: water (70:30 v/v, pH 3.0) and a 1.0 mL min−1 flow rate. The detection wavelength was selected at 210 nm using photo diode array detector and column temperature was optimized to 30 °C. Linearity was obtained at different concentration ranges for all working pharmaceutically active compounds between 0.5 and 25 μg mL−1. The proposed methods were extensively validated according to USP 27 requirements and ICH guidelines. The methods were applied to the analysis of pharmaceutical dosage forms containing binary mixtures of enalapril–lercanidipine and enalapril–nitrendipine. Moreover, the proposed methods were applied for the degradation studies of the selected compounds. Degradation studies were conducted using stress conditions such as UV light, acidic and alkaline hydrolysis, oxidation and heat in oven, to evaluate the ability of the separation of the response of standard compounds from their degradation products.