Assessment of Structural Compatibility of Saxagliptin in Physical Mixtures with some excipient by Using HPLC

2020 ◽  
Vol 16 (8) ◽  
pp. 1074-1082
Author(s):  
Sachin B. Gurav ◽  
Neela M. Bhatia
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Compatibility Study ◽  
Solid States ◽  
Related Substances ◽  
Ich Guidelines ◽  
Liquid Chromatographic ◽  
Physical Mixtures ◽  
Excipient Compatibility

Introduction: Saxagliptin hydrochloride is an oral hypoglycemic agent used for the treatment of type 2 diabetes mellitus. Saxagliptin is unstable because it undergoes an intra-molecular cyclisation reaction to form a cyclicamidine in both solution and solid states. In pharmaceutical development of saxagliptin it is important to select the excipients which are compatible and help to minimize the formation of cyclicamidine. In excipient compatibility study for saxagliptin it is essential to identify the formation of cyclicamidine and other related substances. Materials and Methods: In the current work, the method for quantification of saxagliptin, cyclicamidine and its related substances by high performance liquid chromatographic was developed and validated. This method was used as screening technique for assessing the compatibility of saxagliptin with some pharmaceutical excipients. These were evaluated by analyzing the pure saxagliptin and saxagliptin- excipient in physical mixture, which were stored under different conditions at 40°C/75% Relative Humidity (RH) for one month. The method was successfully validated as per ICH guidelines. Results and Conclusion: The results of compatibility study demonstrate the suitability of saxagliptin with Methocel, Polyethylene Glycol (PEG), Opadry Red, Opadry pink, Opadry white, and Opadry Pink.

RP-HPLC METHOD FOR ESTIMATION OF LORNOXICAM IN TABLETS AND IN DISSOLUTION SAMPLES USING MASS SPECTROMETRIC COMPATIBLE BUFFERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Mass Spectrometric ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

scholarly journals Validation of high-performance liquid chromatographic method for analysis of fluconazole in microemulsions and liquid crystals

2014 ◽  
Vol 50 (2) ◽  
pp. 381-389 ◽  
Author(s):  
Hilris Rocha e Silva ◽  
Fernanda Kolenyak dos Santos ◽  
Gabriela Marielli da Luz ◽  
Marlus Chorilli ◽  
Maria Palmira Daflon Gremião
Keyword(s):  
Liquid Crystals ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Fungal Diseases ◽  
Cutaneous Lesions ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Site Of Action ◽  
Copaiba Oil ◽  
Liquid Chromatographic

In recent decades, there has been a significant increase in the incidence of fungal diseases. Certain fungal diseases cause cutaneous lesions and in the usual treatment, generally administred orally, the drug reaches the site of action with difficulty and its concentration is too low. An approach much explored in recent years is the development of nanotechnology-based drug delivery systems, and microemulsions (ME) and liquid crystals (LC) are promising. ME and LC were developed with oleic acid or copaiba oil as the oil phase, propoxyl (5OP) ethoxyl (20 OE) cetyl alcohol as surfactant and water. An analytical method to assess the incorporation of fluconazole (FLU) in the systems under study was validated according to guidelines of the International Conference on Harmonization (ICH) guidelines and the Brazilian Food, Drug and Sanitation Agency (ANVISA). The method was conducted on a C18-RP column (250 × 4.6 mm i.d.), maintained at room temperature. The mobile phase consisted of acetonitrile and water (50:50, v/v), run at a flow rate of 1.0mL/min and using ultraviolet detection at 210nm. The chromatographic separation was obtained with a retention time of 6.3min, and was linear in the range of 20-400 µg/mL (r2=0.9999). The specificity showed no interference of the excipients. The accuracy was 100.76%. The limits of detection and quantitation were 0.057 and 0.172 µg.mL-1, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the incorporation of FLU in ME and LC, contributing to improve the quality control and to assure the therapeutic efficacy.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

scholarly journals Stability Indicating HPLC-ECD Method for the Analysis of Clarithromycin in Pharmaceutical Dosage Forms: Method Scaling versus Re-Validation

2019 ◽  
Vol 87 (4) ◽  
pp. 31 ◽  
Author(s):  
Makoni ◽  
Chikukwa ◽  
Khamanga ◽  
Walker
Keyword(s):  
High Performance ◽  
The United States ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Analytical Column ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Run Time ◽  
Liquid Chromatographic

An isocratic high-performance liquid chromatographic method using electrochemical detection (HPLC-ECD) for the quantitation of clarithromycin (CLA) was developed using Response Surface Methodology (RSM) based on a Central Composite Design (CCD). The method was validated using International Conference on Harmonization (ICH) guidelines with an analytical run time of 20 min. Method re-validation following a change in analytical column was successful in reducing the analytical run time to 13 min, decreasing solvent consumption thus facilitating environmental and financial sustainability. The applicability of using the United States Pharmacopeia (USP) method scaling approach in place of method re-validation using a column with a different L–designation to the original analytical column, was investigated. The scaled method met all USP system suitability requirements for resolution, tailing factor and % relative standard deviation (RSD). The re-validated and scaled method was successfully used to resolve CLA from manufacturing excipients in commercially available dosage forms. Although USP method scaling is only permitted for columns within the same L-designation, these data suggest that it may also be applicable to columns of different designation.

scholarly journals HPLC method for the development and validation of busulfan in pharmaceutical formulation

2021 ◽  
Vol 6 (3) ◽  
pp. 136-142
Author(s):  
K Swamy Sekhar ◽  
Ch Venkata kishore ◽  
V Tejeswara Rao ◽  
K. Raghu Babu
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Detector Response ◽  
Control Analysis ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
System Controller

A validated HPLC method was developed for the determination of Busulfan (BUS) in pharmaceutical formulation.It is a new simple, accurate, precise and reproducible HPLC method has been developed for the estimation of Busulfan (1,4-butanediol dimethanesulfonate) in its inject able dosage.The method developed in High Performance Liquid Chromatographic method using suitable column (YMC Pack ODS-A (150 x 4.6) mm, 3µm). All the components of the system are controlled using SCL-10Avp System Controller. Data acquisition was done using LC Solutions software.The method was validated as per the ICH guidelines. Thus, the proposed HPLC method can be successfully applied for the routine quality control analysis of formulations. The method developed is simple and is better than the methods reported in the literature and the method is capable to give a good detector response, the recovery calculated was within the range of 98% to 102% of the specification limits.

scholarly journals Simple, Accurate and Efficient High Performance Liquid Chromatographic Method for Determination of Vandetanib in Bulk and in Pharmaceutical Forms

2021 ◽  
pp. 153-160
Author(s):  
M. Murali ◽  
P. Venkateswara Rao
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, selective, linear, precise and accurate isocratic RP-HPLC method was developed and validated for rapid assay of Vandetanib, an anticancer drug, in both bulk and tablet dosage form. Elution at a flow rate of 1ml/min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of acetonitrile, water and orthophosphoric acid in the ratio of 90:08:02 (v/v/v). Linearity was observed in concentration range of 50-200 ppm. The retention time for Vandetanib was 3.326 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Vandetanib in pharmaceutical dosage forms. Moreover the detection alone was also verified through LC-MS of the Vandetanib drug using ESI method which provides future scope for study of this drug using LC-MS method also.

VALIDATION OF THE QUALITATIVE DETERMINATION OF HPLC METODS FOR SUCROSE AND PEG-2000-DSPE IN A LIPOSOMAL FORM OF THE PHOTOSENSITIZER LIPOPHTHALOCYAN

2020 ◽  
pp. 241-244
Author(s):  
ANNA LANTSOVA ◽  
EKATERINA SANAROVA ◽  
MARIA DMITRIEVA ◽  
OLGA ORLOVA ◽  
NATALIA OBOROTOVA ◽  
...  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Statistical Parameters ◽  
Liposomal Form ◽  
True Value ◽  
Ich Guidelines ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic ◽  
Qualitative Determination

Objective: This study was undertaken with the aim of the validate the simple isocratic metods high-performance liquid chromatographic (HPLC) for the estimation of PEG-2000-DSPE and sucrose in liposomal medicinal formulations of the phthalocyanine photosensitizer Lipophthalocyan. Methods: HPLC quantification was carried out by using of YMC-Pack Polyamine II column. The mobile phase (for sucrose: acetonitrile: water: ethyl acetate in the ratio of 450: 200: 20; for PEG-2000-DSPE: water in the ratio 10: 90) was pumped at a flow rate of 1 ml/min. Following the guidelines of the International Conference on Harmonization (ICH), the methods was validated for various analytical parameters like specificity, linearity, detection limit, quantitative limit, correctness, and accuracy. Results: The obtained results of the analysis were validated statistically. The correlation coefficient for the linearity was 0.999292, for sucrose, and 0.997650 for PEG-2000-DSPE. The methods can be assessed as correct, as the results obtained are close to the true value and the confidence interval for both methods include 100%. The coefficients of variation in both methods in determining the accuracy were less than 3%. Conclusion: The proposed HPLC methods were validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed methods are sensitive, precise, reliable and simple for the estimation of PEG-2000-DSPE and sucrose in Lipophthalocyan.

Theophylline Determination in Pharmaceuticals Using a Novel High-performance Liquid Chromatographic Process

2021 ◽  
Vol 19 (7) ◽  
pp. 196-208
Author(s):  
H.N.K. AL-Salman ◽  
Ekhlas Qanber Jasim ◽  
Hussein H. Hussein
Keyword(s):  
High Performance ◽  
Orthophosphoric Acid ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
International Conference ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Chromatographic Process ◽  
Liquid Chromatographic

Objective: The current study aims to find a suitable, accurate, and faster RP-HPLC technique for the determination of theophylline, which could then be validated in accordance with the International Conference on Harmonization (ICH) guidelines. The Aim of this Study: The aim of this study was to develop an efficient, accurate, and faster RP-HPLC method for determining theophylline, which was then validated using the International Conference on Harmonization (ICH) guidelines. Methods: In the HPLC analysis, the Waters 2695 was used. The drug was isolated better using an Ion Pac zorbax 300-SCX Agilent Column, 5 m, 4.6 250 mm, with a liquid phase of Orthophosphoric acid (0.1 percent Orthophosphoric acid in HPLC acetonitrile and Methanol in the ratio of 50:50 v/v at a flow rate of 1ml/min, with discovery at 280 nm using a PDA detector. Results: Theophylline's preservation time was discovered to be 3.747 0.127 min. In the 5-25 mg/l range, the procedure was found to be linear, with a parallel coefficient (R2) of 0.9998. The LOD and LOQ of the system were determined to be (0.99 and 3) g/ml, respectively. The technique and system precisions were predicted using, and the outcomes were determined as percent RSD principles, which were noticed to be within the strict limitations. Theophylline recovery was detected to be in the 99-100 percent range, confirming the method's precision. Conclusion: Using basic ICH guidelines, the suggested RP-HPLC process was validated. The following methodology can be used successfully and easily for routine diagnostic analysis.

High-performance liquid-chromatographic determination of free nicotinic acid and its metabolite, nicotinuric acid, in plasma and urine.

1978 ◽  
Vol 24 (10) ◽  
pp. 1740-1743 ◽  
Author(s):  
N Hengen ◽  
V Seiberth ◽  
M Hengen
Keyword(s):  
Nicotinic Acid ◽  
High Performance ◽  
Isonicotinic Acid ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Related Substances ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract We report a liquid-chromatographic procedure for determining free nicotinic acid and a metabolite, nicotinuric acid, in plasma and urine. Five-tenths milliliter of urine or deproteinized plasma is evaporated and the residue analyzed isocratically by reversed-phase ion-pair chromatography, with measurement of the eluted nicotinic acid and nicotinuric acid at 254 nm. Nicotinic acid, nicotinuric acid, and the internal standard (isonicotinic acid) have retention times of 7.8, 8.4, and 6.8 min, respectively, in plasma, and 12.3, 13.1, and 10.8 min in urine, because of double column length. Day-to-day reproducibilities (CV) for nicotinic acid and nicotinuric acid within 7.5% are attainable for the concentration ranges 0.1--20 mg/liter, equivalent to 0.81--162 micromol of nicotinic acid and 0.55--11 micromol of nicotinuric acid per liter for plasma; in urine for the range 0.5--100 mg/liter, equivalent to 4--810 micromol of nicotinic acid and 2.8--555 micromol of nicotinuric acid per liter. Metabolites of nicotinic acid such as nicotinamide, N-methylnicotinamide, 2-hydroxypyridine-5-carboxylic acid, and other structurally related substances do not interfere.

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