scholarly journals New HPLC method for in vitro dissolution study of antihypertensive mixture amlodipine and perindopril using an experimental design

2013 ◽  
Vol 11 (5) ◽  
pp. 717-724
Author(s):  
Anna Gumieniczek ◽  
Paulina Mączka ◽  
Tadeusz Inglot ◽  
Rafał Pietraś ◽  
Elżbieta Lewkut ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Column Temperature ◽  
Dissolution Study ◽  
Burman Design ◽  
First Time ◽  
Plackett Burman Design

AbstractA new HPLC method was developed for the determination of amlodipine and perindopril in their binary mixture as a part of a routine control of combined formulations. For the first time an HPLC method was used for an in vitro dissolution study of tablets containing the above drugs. The presented method was validated to meet official requirements and this validation included specificity, stability, linearity, precision and accuracy. Chromatography was carried out using a LiChrospher RP-18 column, a mixture containing acetonitrile and phosphate buffer of pH 3.0 (50:50, v/v) as mobile phase and UV detection at 225 nm. The dissolution test was performed using 900 mL of phosphate buffer at pH 5.5 containing 1% cetylpyridini chloride (CPC) at 37°C and 75 rpm, using the paddle method. Robustness procedure was done according to the plan defined by the Plackett-Burman design. The effects of acetonitrile content, pH of the buffer and flow rate of the mobile phase, column temperature, pH and CPC content in the dissolution medium as well as rotation speed of the paddle were considered. After that, both graphical and statistical methods were used for identification of significant and non-significant effects.

Formulation and Evaluation of Microbially- triggered tablets of Valdecoxib

2010 ◽  
Vol 2 (1) ◽  
Author(s):  
Surender Verma ◽  
S. Singh ◽  
D. Mishra ◽  
Atul Gupta ◽  
Rakesh Sharma
Keyword(s):  
Phosphate Buffer ◽  
Guar Gum ◽  
Oral Route ◽  
Matrix Tablets ◽  
In Vitro Dissolution ◽  
Wet Granulation ◽  
Dissolution Study ◽  
Caecal Content ◽  
Model Drug

The objective of present study was to develop colon targeted drug delivery using bacterially triggered approach through oral route. Valdecoxib (COX-2 inhibitor) was chosen as a model drug in order to target it to colon which may prove useful in inflammatory bowel disease and related disorders. Matrix tablets of Valdecoxib were prepared by wet granulation technique utilizing different ratio of Guar gum and Sodium starch glycholate. The prepared matrix tablets were evaluated for uniformity of weight, uniformity of content, hardness and in vitro dissolution study in simulated gastric and intestinal fluid (Phosphate Buffer pH-1.2, pH-6.8 and pH-7.4), followed by Dissolution study in bio-relevant dissolution media Phosphate Buffer (pH-6.8) containing rat caecal content. The results revealed that the formulated batch had released lesser quantity of drug at pH 1.2 and pH 7.4 in 2 hors whereas in biorelevent dissolution media containing rat caecal content it released significantly higher amount of drug which was also significantly higher than the dissolution media of same pH without caecal content (microflora) and it was concluded that guar gum can be used as a potential carrier for targeting drugs to colon.

scholarly journals Development and application of a validated HPLC method for the analysis of dissolution samples of mexiletine hydrochloride capsules

2010 ◽  
Vol 75 (7) ◽  
pp. 975-985 ◽  
Author(s):  
Dragan Milenovic ◽  
Zoran Todorovic
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Uv Detection ◽  
In Vitro Dissolution ◽  
Selective Method ◽  
Dissolution Studies ◽  
Detection And Quantification

The aim of this work was to develop and validate a simple, efficient, sensitive and selective method for the analysis of dissolution samples of mexiletine hydrochloride capsules by HPLC without the necessity of any time-consuming extraction, dilution or evaporation steps prior to drug assay. Separation was performed isocratically on a 5 ?m LiChrospher 60, RP-Select B column (250 x 4 mm ID) using the mobile phase buffer-acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1 and UV detection at 262 nm. The elution occurred in less than 10 minutes. The assay was linear in the concentration range 50-300 ?g mL-1 (r2 = 0.9998). The validation characteristics included accuracy, precision, linearity, specificity, limits of detection and quantification, stability, and robustness. Validation acceptance criteria were met in all cases (the percent recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The method could be used for the determination of mexiletine hydrochloride and for monitoring its concentration in in vitro dissolution studies.

scholarly journals Solubility Enhancement and Pharmacokinetic Assessment of Chemically Modified Lamotrigine in Rat Blood Plasma by HPLC

2019 ◽  
pp. 1-16
Author(s):  
Krishna R. Gupta ◽  
Ashok R. Gautam ◽  
Anvesha V. Ganorkar ◽  
Milind J. Umekar
Keyword(s):  
Oral Administration ◽  
Rat Plasma ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Standardization Method ◽  
Reverse Phase ◽  
Dissolution Study ◽  
Solubility Study ◽  
Internal Standardization

Aims: Synthesis/preparation of Lamotrigine (LMN) complexes with β-CD, Caffeine, Nicotinamide, EDTA and Development of a new reverse phase liquid chromatographic (HPLC) method for the investigation of Lamotrigine in rat plasma after oral administration and pharmacokinetic assessment of Lamotrigine. Study Design: The present work describes the formation of LMN drug complexes with β-Cyclodextrin, Caffeine, Nicotinamide and Disodium EDTA. Physical mixture, kneading and solvent evaporation methods were used to prepare LMN complexes (In ratios 1:1, 1:2, 2:1). Further characterization was performed by UV, FTIR, PXRD, and DSC. A reverse phase HPLC method was developed for the investigation of LMN in rat plasma using internal standardization method after oral administration of LMN and its complexes. Place and Duration of Study: Department of Pharmaceutical Chemistry, Smt. Kishoritai Bhoyar College of Pharmacy, RTMN University, Nagpur, between July 2018 and June 2019. Methodology: LMN complexes with β-CD, Caffeine, Nicotinamide, EDTA was prepared in three ratios i.e. 1:1, 1:2 and 2:1 and characterized by UV, FTIR, PXRD, and DSC. In-vitro Solubility study was performed by saturation solubility study, further % practical yield, drug content, melting point was determined. In-vitro dissolution study of prepared complexes was performed in dissolution apparatus using the paddle method, according to USP Type II. Dissolution studies were carried out using 900 mL 0.1M HCl at 37± 0.5°C at 50 revmin−1 (US FDA guidelines).The interaction of LMN with these hydrophilic complexing agents was characterized by UV, FTIR, PXRD and DSC. A reverse phase HPLC bioanalytical method was developed and validated as per ICH guidelines for the quantitative determination of LMN in rat plasma using internal standardization method (HTZ) after oral administration of LMN and its complexes. The method was successfully applied for the pharmacokinetic study in rat. The pharmacokinetic parameter like AUCt, AUCi, MRTi, Cmax, Tmax, t1/2, were calculated using pharmacokinetic software PK solver 2. The efficient separation was carried out for High Performance Liquid Chromatography (HPLC) method on Eclipse XDB-C18 (150×4.6×5 µ) column using a mobile phase consisting of filtered and degassed mixture of potassium dihydrogen orthophosphate buffer (pH 7.0) and Methanol in the ratio 65:35 v/v at a flow rate of 0.8 mL/min and UV detection at 307 nm. Results: The LMN complexes were successfully prepared and characterized by UV, FTIR, PXRD, and DSC from which solvent evaporation method was found to be best as per result of in-vitro dissolution study. In-vitro dissolution study reveals that LMN-Caffeine (C1) and LMN-NTM (N1) complexes showed 100.14 and 100.01% drug release at 15 min and 20 min respectively as compared to pure drug (LMN) which shows only 50.56% drug release at 75 min. LMN concentration in blood plasma reached (Cmax) was found to be 19.4732 µg/mL at Tmax of 5h, Whereas Cmax of LMN complexes were found to be 48.4876 (B1), 72.2160 (C1), 62.2739 (N1) and 49.3170 (E1) µg/mL at Tmax of 5h out of which complex C1 and N1 in the present study resulted in a sharp increase in Cmax. All complexes showed 4 to 5 time enhancement of Cmax as compared to LMN.. The results demonstrated that complexes of Lamotrigine were successful strategy to improve the solubility and dissolution behavior of Lamotrigine. The complex B1 shows maximum t1/2 and MRTi of 36.224 h and 52.441 h as compared to C1, N1 and E1 having t1/2 of 14.1575, 16.258 and 21.702 h and MRTi  of 19.997, 22.994 and 30.883 h respectively. Hence B1 required lesser dosing frequency as compared to other complexes. Conclusion: The Lamotrigine complexes were prepared and confirmation of prepared complexes was done by physical characterization (FTIR. DSC, PXRD and UV) and solubility determination by saturation solubility study. The bioanalytical method was developed for estimation of plasma drug concentration of LMN. The method was validated according to ICH guidelines to estimate the mean plasma concentration of LMN after oral administration using internal standardization method (HTZ). Method was reproducible and high recovery of LMN from its complexes was achieved. The method was found to be highly satisfactory sensitive, accurate, linear and specific.

Validation of RP-HPLC Method for Determination of Omeprazole in Dissolution Media and Application to Study in-vitro Release from Solid-SNEDDS

2021 ◽  
Vol 17 ◽  
Author(s):  
Suhair S. Al-Nimry ◽  
Khouloud A. Alkhamis ◽  
Bashar M. Altaani
Keyword(s):  
Dissolution Rate ◽  
Phosphate Buffer ◽  
Water Solubility ◽  
In Vitro Release ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Limit Of Quantification ◽  
Rp Hplc

Background: Omeprazole has poor water solubility, is unstable in acidic solutions, and undergoes first pass metabolism which results in lowering its bioavailability. A solid Self-Nano Emulsifying Drug Delivery System (SNEDDS) was previously prepared to enhance its dissolution. Objective: Development and validation of a RP-HPLC method with UV detection for the determination of omeprazole in 0.1N HCl and in 0.01 M phosphate buffer (pH 7.4). Methods: Validation was according to the ICH Q2 (R1) guidelines in terms of linearity, accuracy and precision, lower limit of quantification, sensitivity, specificity, and robustness. The developed and validated method was used to study the in-vitro dissolution of the drug from the solid-SNEDDS, commercial products and of the unprocessed drug. The dissolution was studied in 500 ml of 0.1N HCl during the first 2 hours, and 900 mL of 0.01 M phosphate buffer (pH 7.4) during the last hour (37 ± 0.5 oC and 100 rpm). Results: The method was linear in the range 1-50 μg/ml, accurate and precise as indicated by the ANOVA test. It was specific to the drug and the pharmaceutical excipients did not affect the determination of its concentration. The method was robust to small changes in pH, composition, and flow rate of the mobile phase. The dissolution rate of omeprazole from the Solid-SNEDDS was faster than that from two commercial dosage forms and than the dissolution rate of the unprocessed drug. Conclusion: The method met the acceptance criteria and was applied successfully in studying the rate of dissolution of the drug.

scholarly journals Chemometrically assisted RP-HPLC method development for efficient separation of ivabradine and its eleven impurities

2020 ◽  
Vol 32 (1) ◽  
pp. 53-63 ◽  
Author(s):  
Jovana Tomić ◽  
Branka Ivković ◽  
Slavica Oljačić ◽  
Katarina Nikolić ◽  
Nevena Maljurić ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Chromatographic Retention ◽  
Positional Isomers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Efficient Separation ◽  
Rp Hplc

The aim of this study was to develop a novel reversed-phase high-performance liquid chromatography (RP-HPLC) method for efficient separation of ivabradine and its 11 impurities. Similar polarity of impurities in the sample mixture made method optimization challenging and accomplishable only when different chemometric tools, such as principal component analysis (PCA), Box–Behnken design (BBD), and desirability function as a multicriteria approach, were employed. The presence of 3 positional isomers (impurities III, V, and VI), keto–enol tautomerism of impurity VII, and diastereoisomers of impurity X made separation of this complex mixture even more challenging. Chromatographic retention parameters obtained with the mobile phase consisting of 30 mM phosphate buffer and acetonitrile (80:20, v/v) on four different RP-HPLC columns at varying pH values (3.0, 4.0, and 5.0) were subjected to the PCA analysis to select the column with the most appropriate selectivity. Then the column temperature, pH of the aqueous component of mobile phase, phosphate buffer molarity and the organic solvent content in the mobile phase were estimated employing BBD. Valid and reliable mathematical models towards resolution of twelve critical peak pairs were obtained. After determination of the desirability making criteria for all responses, desirability functions were established and used in optimization. The proposed optimal chromatographic conditions included the Zorbax Eclipse Plus C18 chromatographic column (100 × 4.6 mm, 3.5 μm), the column temperature of 34 °C, the mobile phase flow rate of 1.6 mL min−1 and the UV detection at 220 nm. The mobile phase consisted of the 28 mM phosphate buffer at pH 6.0 and acetonitrile (85:15, v/v). Separation of one pair of positional isomers was not achieved, so methanol was added to the organic part of mobile phase in small increments with the optimal ratio of methanol to acetonitrile 59:41, v/v. The overall organic component of the mobile phase also increased to 18%, accelerating the chromatographic analysis.

scholarly journals Multivariate optimization of liquid chromatographic conditions for determination of dapagliflozin and saxagliptin, application to an in vitro dissolution and stability studies

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Sunitha Gurrala ◽  
Shiva Raj ◽  
C. V. S. Subrahmanyam ◽  
Panikumar D. Anumolu
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
In Vitro Dissolution ◽  
Simultaneous Estimation ◽  
Stability Studies ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Form

Abstract Background Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase. Results Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/mL for saxagliptin, respectively. Conclusion The proposed method was exploited for assay, in vitro dissolution, and stability studies of target drugs in marketed dosage form.

scholarly journals A Fast and Validated HPLC Method for Simultaneous Determination of Dopamine, Dobutamine, Phentolamine, Furosemide, and Aminophylline in Infusion Samples and Injection Formulations

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Fuchao Chen ◽  
Baoxia Fang ◽  
Sicen Wang
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Precision Data ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
The Stability

A simple, fast, and validated HPLC method was developed for the simultaneous quantization of five cardiovascular agents: dopamine (DPM), dobutamine (DBM), phentolamine (PTM), furosemide (FSM), and aminophylline (APL) either in infusion samples or in an injection dosage form. The proposed method was achieved with a 150 mm × 4.6 mm, 5.0 μm C18 column, by using a simple linear gradient. Mobile phase A was buffer (50 mM KH2PO4) and mobile Phase B was acetonitrile at a flow rate of 1.0 mL/min. The column temperature was kept at 30°C, and the injection volume was 20 μL. All analytes were separated simultaneously at a retention time (tr) of 3.93, 5.84, 7.06, 8.76, and 9.67 min for DPM, DBM, PTM, FSM, and APL, respectively, with a total run time of less than 15.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 12.0–240.0, 12.0–240.0, 20.0–200.0, 6.0–240.0, and 10.0–200.0 μg/mL DPM, DBM, PTM, FSM, and APL, respectively. Interday and intraday accuracy and precision data were recorded in the acceptable limits. The new method has successfully been applied for quantification of all five drugs in their injection dosage form, infusion samples, and for evaluation of the stability of investigated drugs in mixtures for endovenous use. The results of the stability study showed that mixtures of DPM, DBM, PTM, FSM, and APL in 5% glucose or 0.9% sodium chloride injection were stable for 48 hours when stored in polypropylene syringes at 25°C.

In vitro dissolution study of plutonium in aerosol particles from the Mayak PA: a tool for individualised dose estimates

2007 ◽  
Vol 127 (1-4) ◽  
pp. 60-63 ◽  
Author(s):  
E. E. Aladova ◽  
S. A. Romanov ◽  
R. A. Guilmette ◽  
V. F. Khokhryakov ◽  
K. G. Suslova
Keyword(s):  
Aerosol Particles ◽  
In Vitro Dissolution ◽  
Dissolution Study

scholarly journals A New Validated Stability Indicating RP-HPLC Method for Simultaneous Quantification of Formoterol Fumarate Dihydrate and Mometasone Furoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (11) ◽  
pp. 2723-2728
Author(s):  
Surya Prakash Mamillapalli ◽  
Gourabattina Lakshmi Prasanna ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Metered Dose ◽  
Formoterol Fumarate ◽  
Dose Inhalation

Stability indicating reversed phase-HPLC method for simultaneous estimation of mometasone furoate (MAF) and formoterol fumarate (FFD) in metered dose inhalation aerosol (MDI) dosage formulation has been developed and discussed in the present work. The chromatographic separation was achieved using Hypersil ODS column (250 mm × 4.6 mm, 3 μm) using an isocratic separation mode at a flow rate of 1.2 mL/min, column temperature of 50 ºC. The system operates with a mobile phase comprising of solution-A (buffer): Solution-B (acetonitrile) mixed in the ratio of 70:30 %v/v at a UV detection wavelength of 214 nm. Retention times of mometasone furoate and formoterol fumarate found to be about 3 min and 7 min, respectively. All possible degradation products of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector. Both analyte were subjected to force degradation studies, found all degradants were resolved from analyte peaks and also other process-related impurities. The proposed method is validated for specificity, linearity, accuracy, precision and robustness as per ICH guidelines and found to be adequate. Method stood to be robust with variation in column temperature, flow rate, pH of buffer and organic content in mobile phase.

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