scholarly journals Analytical Method Development Using Central Composite Design for Estimation of Lamotrigine in Lipid Nanoformulation

2020 ◽  
Vol 57 (1) ◽  
pp. 223-235
Author(s):  
Puja K Gangurde ◽  
Navya Ajitkumar Bhaskaran ◽  
Ruchi Verma ◽  
JOBIN Jose ◽  
Lalit Kumar
Keyword(s):  
Central Composite Design ◽  
Flow Rate ◽  
Retention Time ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Coefficient Of Determination ◽  
Uv Detector ◽  
Relative Standard ◽  
Central Composite

Objective of this study was to develop and validate HPLC-UV method for detection of LTG in lipid nanoformulations. HPLC-UV method was developed according to ICH Q2(R1) guidelines. Central composite design was used effectively to optimize and study the effect of buffer strength, flow rate, pH of buffer and mobile phase composition on responses such as tailing factor, peak area, retention time and number of theoretical plates. The 30 mM ammonium formate buffer and acetonitrile (in the ratio 65:35 %v/v) was used as mobile phase in the study. The mobile phase was delivered at the flow rate of 1.0 mL/min. The detection of buffer was performed at 256 nm using UV detector. The drug entrapment of prepared formulation was also determined using developed HPLC method. Retention time of lamotrigine was found to be 3.844 min. The coefficient of determination (r2) value from linearity was found to be 0.9982. Percent relative standard deviation value of precision was found to be within the acceptable range. The estimated LOD and LOQ were found to be 9.07 ng/mL and 27.48 ng/mL, respectively. Drug entrapment of prepared lipid nanoformulation was found to be 73.44 � 6.65%. The results conclude that the developed analytical method is simple, precise, sensitive, fast and reproducible. Applications of developed method for determination of drug entrapment in prepared lipid nanoformulation confirmed that the developed analytical method is suitable for estimation of lamotrigine in lipid nanoformulations.

scholarly journals CENTRAL COMPOSITE DESIGN APPLIED IN HPLC OPTIMIZATION FOR ANALYSIS OF TARTRAZINE AND AURAMINE O IN POWDER DRINKS

2019 ◽  
pp. 211-215
Author(s):  
ANNISA DYAH LESTARI ◽  
Abdul Rohman ◽  
SUDIBYO MARTONO
Keyword(s):  
Central Composite Design ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Acetate Buffer ◽  
Ammonium Acetate Buffer ◽  
Acetate Concentration ◽  
Rp Hplc ◽  
Central Composite

Objective: This study was intended to optimize reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of Tartrazine (TAR) and Auramin O (AUO) in powder drinks using experimental design of central composite design (CCD) approach. Methods: TAR and AUO in powder drink product has same properties, therefore both analytes were analysed using C18 column (XBridge Shield RP 18 250 mm x 4.6 mm i.d., 5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. Some factors responsible for RP-HPLC separation of TAR and AUO including the concentration of buffer, the ratio of mobile phase and flow rate were optimized using CCD. The responses evaluated were peak area, retention time, and tailing factor. The mobile phase used was acetonitrile and ammonium acetate buffer, and acetonitrile composition was optimized at 84-86% for separation of TAR and AUO, delivered at a flow rate of 0.8–1.2 ml/min, using ammonium acetate buffer at 19-21 mmol. Results: CCD showed that separation of TAR and AUO was influenced by flow rate, the ratio of acetonitrile and ammonium acetate concentration. These factors affected significantly to retention time, peak area, and tailing factor. The optimal condition obtained based on CCD was flow rate of 1.2 ml/min, the ratio of acetonitrile 86%, and ammonium acetate concentration of 19 mmol. Conclusion: CCD can be used to get optimum condition for analysis of TAR and AUO in powder drink product.

scholarly journals Stability Kinetics of Imiquimod: Development and Validation of an Analytical Method

2019 ◽  
Vol 57 (7) ◽  
pp. 583-591
Author(s):  
Mandeep Sharma ◽  
Gajanand Sharma ◽  
Bhupinder Singh ◽  
O P Katare
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Volume Ratio ◽  
Coefficient Of Determination ◽  
Calibration Plot ◽  
Dependent Manner ◽  
Uv Detector ◽  
Concentration Dependent Manner ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract For a new immune modulator imiquimod, various liquid chromatography methods have been described in literature but all of them are deficient in one or other aspects of complete method development. The present work intends to develop and validate the stability indicating reverse phase high performance liquid chromatographic (HPLC) method. The isocratic flow of mobile phase comprising equal volume ratio of acetate buffer BP pH 3.7 and acetonitrile at the rate of 1.5 mL/min through the C-18 column at 25°C lead to elution of drug around 2.3 min when analyzed at 244 nm using UV-detector. The linear regression equation in calibration plot was y = 61632×-1224 with 0.9992 coefficient of determination (r2). The percent relative standard variation (% RSD) in peak area at low, mid and high region of linearity range was less than 5% in precision studies. The method was able to detect 0.039 μg/mL of drug but practical limit of quantitation (LOQ) was 1.5 μg/mL. The imiquimod molecule was stable in all except oxidizing conditions where it degraded into more polar molecule in hydrogen peroxide (H2O2) concentration dependent manner. Therefore, an analytical method capable of accurately and specifically estimating the drug in microgram range was successfully developed.

STABILITY INDICATING LIQUID CHROMATOGRAPHIC ASSESSMENT OF DOLUTEGRAVIR BY AQBD APPROACH – CENTRAL COMPOSITE DESIGN

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (10) ◽  
pp. 44-51
Author(s):  
G. Sunitha ◽  
◽  
P. D Anumolu ◽  
C.V.S Subrahmanyam ◽  
G Mounika ◽  
...  
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Values ◽  
Mass Spectral ◽  
Theoretical Plates

Based on the current regulatory requirements for analytical method development, a RP-HPLC method for quality control of dolutegravir in dosage form has been optimized using analytical quality by design (AQbD) approach. Experimental observations were analysed by full factorial experimental design in Sigmatech software with two variables (flow rate and % organic mobile phase) whilst the number of theoretical plates was considered as response. The analytical method conditions were optimized as mobile phase (40:60 % V/V) consisting of acetonitrile and ammonium formate buffer, pH 3.0 pumped at a flow rate of 0.6 mL/min in an isocratic mode on SPOLAR C18 Column (250 x 4.6mm, 5μm) with run time of 15 min. The plot between peak area vs. concentration was rectilinear in the range of 5-30 μg/mL with detection and quantification limit values at 0.01 and 0.3μg/mL, respectively at retention time of 13 min. The predicted data from contour diagram for theoretical plates was verified virtually and it was contented with concrete experimental data. The method was validated as per ICH guidelines. The proposed method was pertinent for assay of marketed dosage form (Tivicay) and further extended to quantify the drug in prevalence of degradation products. Degradation pathways of dolutegravir were postulated and characterized by IR and mass spectral data.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF PERINDOPRIL ERBUMINE AND AMLODIPINE BESYLATE IN BULK AND TABLET DOSAGE FORM BY HPLC

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 32-35
Author(s):  
S. R Pattan ◽  
◽  
A.C Patni ◽  
R.A Mali ◽  
C.J. Patni ◽  
...  
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Amlodipine Besylate ◽  
Perindopril Erbumine ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

The objective of this present work was to develop and validate analytical method for quantitative determination of perindopril erbumine and amlodipine besylate in bulk as well as in tablet formulation. The chromatographic separation of the two drugs was achieved on a Varian Microsorb-MV 100-5 C18 column (150×4.6mm, 10 μm). The mobile phase constituted of acetonitrile: buffer (65:35) and pH adjusted to 2.6 with ortho- phosphoric Acid was delivered at the flow rate 1mL/min. Detection was performed at 210 nm. Separation was completed within 6 min calibration curves were linear with correlation coefficient between 0.99 to 1.0 over the concentration range of 2.5 to 15 µg/mL of perindopril erbumine and 10 to 60 µg/mL of amlodipine besylate The relative standard deviation (R.S.D.) was found <2.3%. The proposed method is precise, accurate, selective and rapid for the simultaneous determination of perindopril erbumine and amlodipine besylate.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

scholarly journals QBD APPROACH TO ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR ESTIMATION OF LENVATINIB IN BULK AND PHARMACEUTICAL FORMULATION

2021 ◽  
pp. 183-188
Author(s):  
SACHIN A. BABAR ◽  
SUDHAKAR L. PADWAL
Keyword(s):  
Central Composite Design ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Factor Screening ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Chromatographic Condition ◽  
Central Composite

Objective: The objective of this research was to develop a simple, very rapid, sensitive, accurate, precise reverse phase High-Performance Liquid Chromatography (RP-HPLC) technique for the estimation of Lenvatinib in bulk and its dosage form. Methods: To perform this study, we employed a central composite design (CCD) to make method robust and effective to create chromatographic database. The factor screening studies were performed using 2-factor 10-runs. The factors were selected as the mobile phase ratio and buffer pH. Results: The desirability value of the optimized model was found to be 0.869 and The optimized chromatographic condition was achieved on Enable C18 analytical column with 0.01M Ammonium acetate buffer pH 3.84: methanol (33.17:66.83 v/v) as the mobile phase and flow rate of 1 ml min-1 and detection wavelength was set to 240 nm. The retention time of Lenvatinib was found to be 5.122 min. Linearity was established for Lenvatinib in the range of 10-50 µg/ml with a correlation coefficient (r2=0.9995). The accuracy values were found to be in the range of 98–102%. Intraday precision and Interday precision were in prescribed (Less than 0.98% RSD). Robustness was found to be less than 1.22% RSD. Conclusion: The proposed method was useful for best analysis of Lenvatinib in Bulk pharmaceutical dosage forms. Central Composite Design was an effective tool for the proposed RP-HPLC method.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF DAPAGLIFLOZIN AND SAXAGLIPTIN BY RP-HPLC

2021 ◽  
pp. 134-143
Author(s):  
Sana Tabassum ◽  
Dr.M.Sathishkumar ◽  
Dr.A.Mallik ◽  
Dr.N.Jyothi
Keyword(s):  
Key Words ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Run Time ◽  
Development And Validation

For the coincident evaluation of Dapagliflozin and Saxagliptin in bulk form; Chromatography was run through Intersil-ODS C18 column (250mm× 4.6mm, 5micron) Mobile phase containing Methanol: Water was pumped through the column in the ratio of 45: 55. The flow rate was 1ml/min. The temperature help was ambient i.e., upto300c. The optimized selected wavelength was 210nm. The retention time of Dapagliflozin and Saxagliptin was found to be 4.707min and6.68 min respectively. The %RSD of Dapagliflozin and Saxagliptin was found to be 0.031 and 0.036 respectively. The values of LOD and LOQ obtained from Dapagliflozin and Saxagliptin was 0.56, 1.69 and 0.57, 1.74 respectively. The retention time was decreased and the run time also decreased, so the method development was simple and economical that can be applied successfully for simultaneous estimation of combination of two anti- diabetic drugs; Dapagliflozin and Saxagliptin. KEY WORDS: Dapagliflozin and Saxagliptin, RP-HPLC.

Optimization of permeate flux produced by solar energy driven membrane distillation process using central composite design approach

2016 ◽  
Vol 74 (1) ◽  
pp. 87-98 ◽  
Author(s):  
Salah T. Bouguecha ◽  
Ali Boubakri ◽  
Samir E. Aly ◽  
Mohammad H. Al-Beirutty ◽  
Mohamed M. Hamdi
Keyword(s):  
Solar Energy ◽  
Central Composite Design ◽  
Flow Rate ◽  
High Energy ◽  
Membrane Distillation ◽  
Design Approach ◽  
Coefficient Of Determination ◽  
P Value ◽  
Permeate Flux ◽  
Central Composite

Membrane distillation (MD) is considered as a relatively high-energy requirement. To overcome this drawback, it is recommended to couple the MD process with solar energy as the renewable energy source in order to provide heat energy required to optimize its performance to produce permeate flux. In the present work, an original solar energy driven direct contact membrane distillation (DCMD) pilot plant was built and tested under actual weather conditions at Jeddah, KSA, in order to model and optimize permeate flux. The dependency of permeate flux on various operating parameters such as feed temperature (46.6–63.4°C), permeate temperature (6.6–23.4°C), feed flow rate (199–451L/h) and permeate flow rate (199–451L/h) was studied by response surface methodology based on central composite design approach. The analysis of variance (ANOVA) confirmed that all independent variables had significant influence on the model (where P-value &lt;0.05). The high coefficient of determination (R2 = 0.9644 and Radj2 = 0.9261) obtained by ANOVA demonstrated good correlation between experimental and predicted values of the response. The optimized conditions, determined using desirability function, were Tf = 63.4°C, Tp = 6.6°C, Qf = 451L/h and Qp = 451L/h. Under these conditions, the maximum permeate flux of 6.122kg/m2.h was achieved, which was close to the predicted value of 6.398kg/m2.h.

Method Development and Validation of Droxidopa by RP-UPLC

2021 ◽  
pp. 2125-2128
Author(s):  
Bharani Pandilla ◽  
K. Chitra ◽  
C. N. Nalini ◽  
Ashok P.
Keyword(s):  
Quantitative Analysis ◽  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Statistical Techniques ◽  
Chromatographic System ◽  
Uv Detector ◽  
Economical Method ◽  
Method Development And Validation ◽  
Development And Validation

A simple, rapid, accurate and economical method has been developed for the quantification of droxidopa by UPLC. The chromatographic system was equipped with Phenomenex column C18 (50mm x 3.0mm, 3µ) as stationary phase and UV detector at 235nm, in conjunction with a mobile phase of buffer: methanol (25:75 % v/v ratio) at a flow rate of 1.0mL/min. Linearity was observed over the concentration range of 100-300µg/mL for droxidopa. The droxidopa peak eluted at 0.35 min. The recovery of Droxidopa was found to be 100.17% - 100.63% respectively. Statistical techniques were employed for the validation of precision, linearity, accuracy, robustness and ruggedness and can be applied for routine analysis. Validation revealed that the developed method was specific, accurate, precise, reliable, robust, reproducible and suitable for the routine quantitative analysis.

scholarly journals STATISTICALLY OPTIMIZED AND BOX-BEHNKEN DESIGN ASSISTED METHOD DEVELOPMENT AND VALIDATION OF AN ANTIPSYCHOTIC MEDICATION OLANZAPINE AND ITS RELATED IMPURITIES BY REVERSE-PHASE HPLC-UV SPECTROSCOPY

2021 ◽  
pp. 241-246
Author(s):  
MD IRSHAD ALAM ◽  
AQUIL-UR-RAHIM SIDDIQUI
Keyword(s):  
Flow Rate ◽  
Antipsychotic Medication ◽  
Related Compound ◽  
Mobile Phase ◽  
Method Development ◽  
Forced Degradation ◽  
Mobile Phase Flow Rate ◽  
Box Behnken Design ◽  
Relative Standard ◽  
Pure Drug

Objective: Statistically designed and Box-Behnken design (BBD) assisted reversed-phase high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed and validated for the identification of an antipsychotic medication Olanzapine and its organic impurities in pure drug along with forced degradation studies. Methods: The present developed method employed BBD optimized chromatographic conditions comprising of an Inertsil ODS 3V analytical column with dimension 250 mm x 4.6 mm and particle size 5µ. The isocratic mobile phase was used as a mixture of monobasic sodium phosphate buffer (0.01 M, pH 6), methanol and acetonitrile in the proportion of 40/30/30, v/v. The mobile phase flow rate and UV λmax was 1 ml/min and 260 nm, respectively. The method was optimized by Box-Behnken design using design expert software, comprising of three factors for Olanzapine for instance flow rate (A), mobile phase composition (B) and pH (C) while resolution between Olanzapine related compound A and Olanzapine related compound B (Y1) and tailing of Olanzapine (Y2) were taken as a response. Results: Application of BBD yielded statistically designed method with excellent quality parameters achieved in terms of linearity with the coefficient of correlation (R2>0.9999), limit of detection (LOD, 0.0023-0.16 µg/ml), the limit of quantification (LOQ, 0.007-0.39 µg/ml), accuracy (99-100%) and precision ((2%, relative standard deviation (%RSD) were evaluated as per latest available procedures. Conclusion: Forced degradation conditions were carried out, demonstrated that the optimized method was stable and no any interfering peaks eluting at the similar retention time of the studied compounds. The method was found to be stable, easy, rugged and robust, could be applied for the similar types of the pure drug.

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