scholarly journals Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities

2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Stability Testing ◽  
Stability Indicating ◽  
Chromatographic Parameters ◽  
Interday Precision ◽  
Calculated Amount

Abstract A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was <1 and <1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of >2 from the nearest peak. Insignificant changes in retention time (<4) and calculated amount (<1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.

scholarly journals QuEChERS-HPLC-DAD method for sulphonamides in chicken breast

2013 ◽  
Vol 49 (1) ◽  
pp. 155-166 ◽  
Author(s):  
Simone Caetani Machado ◽  
Mariane Landin-Silva ◽  
Patrícia Penido Maia ◽  
Susanne Rath ◽  
Isarita Martins
Keyword(s):  
Food Safety ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Chicken Breast ◽  
Quechers Method ◽  
Initial Flow ◽  
The Matrix ◽  
Interday Precision

The development of a QuEChERS-HPLC-DAD method using a Lichrospher 60 RP-Select B column (250 x 4.6 mm x 5 µm) at 40ºC, mobile phase constituted by phosphate buffer:acetonitrile (75:25, v/v) at a initial flow rate of 0.5 mL min-1, increased by 1.2 mL min-1 and at 265 nm is presented for simultaneous determination of sulphadiazine, sulphametoxipiridazine and sulphamethoxazole in chicken breast samples. QuEchERS is inexpensive, fast and easy, and the extraction of the analytes of the matrix was successfully employed. In addition, the method presented linearity, in the range of 25, 50, 100, 150, 175, and 200 µg kg-1, precision, selectivity and sensitivity. The intraday precision (RSD %) for QuEChERS method was between 3.6-10.8 (SDZ), 6.9-14.1 (SPZ) and 1.9-10.9 (SMX) and interday precision (RSD%) was between 1.5-9.7, 1.7-4.1 and 2.1-10.2, respectively. Results of accuracy (bias) were in the range of -8.6 to +11.9 %. Therefore, the validated method is clearly useful for the practical residue monitoring of the drugs evaluated in chicken samples, as all the values were within the acceptable criteria used for food safety. Of 6 samples analyzed, none of them showed contamination of the sulphonamides studied at detectable levels.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals An HPLC method for the determination of digoxin in dissolution samples

2010 ◽  
Vol 75 (11) ◽  
pp. 1583-1594 ◽  
Author(s):  
Miroslav Milenkovic ◽  
Valentina Marinkovic ◽  
Predrag Sibinovic ◽  
Radosav Palic ◽  
Dragan Milenovic
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Stability Testing ◽  
Column Length ◽  
Column Temperature ◽  
Chromatographic Parameters ◽  
The Impact ◽  
Full Factorial ◽  
Phase Column

An HPLC method for digoxin quantification in dissolution samples obtained as per the official British Pharmacopeia (BP) method is presented in this paper. The chromatography was performed at 20 ?C on a Symmetry C18; 3.5 ?m, 75 x 4.6 mm column with water - acetonitrile (72 : 28, v/v), as the mobile phase and UV detection at 220 nm. The method was found to be selective, linear, accurate and precise in the specified ranges. The LOD and LOQ were 0.015 ?g mL-1 and 0.050 ?g mL-1, respectively. Robustness testing was conducted to evaluate the impact of minor changes in the chromatographic parameters (i.e., acetonitrile fraction, flow rate of the mobile phase, column temperature and column length) on the characteristics of the digoxin peak. A. full factorial design (24) was used to investigate the influence of the four variables The presented HPLC method was applied in quality and stability testing of Digoxin tablets 0.25 mg.

scholarly journals Stability-Indicating Validated HPLC Method for Simultaneous Determination of Oral Antidiabetic Drugs from Thiazolidinedione and Sulfonylurea Groups in Combined Dosage Forms

2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Uv Light ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Base Temperature ◽  
Stability Indicating ◽  
Acid And Base

Abstract For type 2 diabetes treatment, combinations of drugs from the thiazolidinedione and sulfonylurea groups are now available in the same tablet or capsule. Therefore, a stability-indicating and validated HPLC method was developed for simultaneous determination of pioglitazone, rosiglitazone, and glipizide in combined dosage forms. The examined drugs were subjected to different conditions such as acid and base, temperature, and UV light, and degradation of pioglitazone and glipizide was observed under thermal and acidic stress. However, selectivity of the presented method for pioglitazone, rosiglitazone, and glipizide assay against their degradation products was confirmed. It was also demonstrated to be robust, resisting small deliberate changes in pH of the buffer, flow rate, and percentage of acetonitrile in the mobile phase. The presented method utilizes a LiChrospher RP18 column (125 4.0 mm), acetonitrile in phosphate buffer at pH 4.3 (40 + 60, v/v) as the mobile phase, and UV detection at 225 nm for pioglitazone/glipizide or 245 nm for rosiglitazone/glipizide. The method was validated with respect to linearity, precision, and accuracy. Finally, the elaborated procedure was applied for the QC of pioglitazone/glipizide and rosiglitazone/glipizide mixtures.

scholarly journals Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Bürge Aşçı ◽  
Şule Dinç Zor ◽  
Özlem Aksu Dönmez
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Food Additives ◽  
Hplc Method ◽  
Soft Drinks ◽  
Phase Ratio ◽  
Potassium Sorbate

Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0), flow rate (1.0–1.4 mL/min), and mobile phase ratio (85–95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 μm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r2>0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

scholarly journals TLC-spectrodensitometric method for simultaneous determination of dapagliflozin and rosuvastatin in rabbit plasma: stability indicating assay and kinetic studies

RSC Advances ◽  
2020 ◽  
Vol 10 (67) ◽  
pp. 40795-40805
Author(s):  
Noha S. Abbas ◽  
Sayed M. Derayea ◽  
Mahmoud A. Omar ◽  
Gamal A. Saleh
Keyword(s):  
Ethyl Acetate ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Kinetic Studies ◽  
Urine Samples ◽  
Plasma Stability ◽  
Rabbit Plasma ◽  
Stability Indicating ◽  
Plasma And Urine Samples

Mixtures of DAPA and ROSV were separated using ethyl acetate : methanol (5 : 0.1 v/v) as mobile phase and applied in plasma and urine samples in addition to stability indicating and kinetic studies.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 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. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

scholarly journals Development and Validation of HPLC Fluorescence and UPLC/DAD Stability-Indicating Methods for Determination of Hepatitis C Antiviral Agent Daclatasvir

2019 ◽  
Vol 102 (4) ◽  
pp. 1125-1131
Author(s):  
Amira H Kamal ◽  
Nahla S Ismail ◽  
Mokhtar M Mabrouk ◽  
Lories I Bebawy ◽  
Mai A Mekky
Keyword(s):  
Fluorescence Detection ◽  
Flow Rate ◽  
Mobile Phase ◽  
Ammonium Phosphate ◽  
Uv Detection ◽  
Array Detector ◽  
Fragmentation Pattern ◽  
Stability Indicating ◽  
Ich Guidelines

Abstract Background: Few stability-indicating chromatographic methods were published for determination of daclatasvir. All used UV detection. Objective: This work aimed to develop rapid, specific, and novel stability-indicating methods using HPLC with fluorescence detection and ultra performance liquid chromatography (UPLC) with UV detection for the determination of daclatasvir in bulk powder and in its dosage form. Methods: The drug was subjected to hydrolysis (acidic and alkaline) as per International Conference on Harmonization (ICH) guidelines. The fragmentation pattern of the drug was studied using LC-MS. Separation was carried out first by HPLC using Thermo BDS Hypersil Phenyl (300 mm × 4 mm, 5 μm) column and a mobile phase consisting of ammonium phosphate buffer (0.02 M) pH 3–methanol (40+60, v/v) at flow rate 1 mL/min. Quantitation was achieved by fluorescence detection at 305 and 457 nm for excitation and emission, respectively. The second method used UPLC equipped with diode-array detector. Acquity BEH C18 (50 mm × 2.1 mm, 1.7 μm) column was used with the same mobile phase at flow rate 0.4 mL/min and detection wavelength at 305 nm. ICH guidelines were used for validation. Results: The mean percentage recovery ± SD values for tablet assay were found to be 101.12 ± 0.655 and 99.78 ± 0.632 by HPLC and UPLC methods, respectively. The assay results showed a good agreement with the reported method. Conclusions: The developed HPLC and UPLC methods provide simple, accurate, and reproducible analysis of daclatasvir without interference from degradates. Highlights: This is the first research using fluorescence detection in a stability-indicating chromatographic method for determination of daclatasvir.

RP-UFLC Method for Estimation of Propafenone in Tablets

2014 ◽  
Vol 7 (4) ◽  
pp. 2671-2676
Author(s):  
Sagar Suman Panda ◽  
Ravi Kumar B V V ◽  
Sasmita Kumari Acharjya ◽  
Kalyani Sahu
Keyword(s):  
Uv Radiation ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Correlation Coefficients ◽  
Tablet Formulation ◽  
Forced Degradation ◽  
Recovery Study ◽  
Isocratic Mode

A simple, precise and accurate RP-UFLC method was developed for determination of propafenone hydrochloride. Separation was carried on an Enable C18G column       (250 mm × 4.6 mm i.d., 5 μm) using methanol: 10 mM TBAHS (95:05, v/v) as mobile phase at flow rate of 1.0 ml/min in isocratic mode. The PDA detection wavelength was 247 nm. The retention time of propafenone was 2.692 min. The method was validated for linearity, specificity, precision, accuracy and robustness as per ICH. The method was linear in the concentration range of 10 – 250 µg/ml with correlation coefficients of 0.999. The LOD and LOQ were 4.5 µg/ml and 9.75 µg/ml, respectively. Average recoveries for recovery study were found to be in the range of 99.73-100.58. R.S.D. values for intraday, interday and system precision were found to be less than 2%. Specificity was established after forced degradation was performed by using HCl, NaOH, H2O2, thermal and UV radiation. The method was applied successfully for estimation propafenone in tablet formulation.   

Development and validation of Stability-indicating RP-UPLC Method for the Simultaneous Determination of Ivacaftor, Tezacaftor and Elexacaftor in bulk and their Formulation

2021 ◽  
Vol 25 (12) ◽  
pp. 107-115
Author(s):  
V.V.S.S.N. Raju Sri Datla ◽  
Manikandan Ayyar
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Drug Product ◽  
Dosage Forms ◽  
Combination Drug ◽  
Ultraviolet Detection ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Development And Validation

A simple reproducible stability indicating RP-UPLC method was developed for the simultaneous determination of Ivacaftor, Tezacaftor and Elexacaftor in their combined dosage forms using HSS C18, 1.8μm, 100mm x2.1 mm i.d. column. A mobile phase of phosphate buffer (10mM) pH-4.8 and acetonitrile in the ratio of 70: 30v/v mixture was used for separation and quantification of ivacaftor, tezacaftor and elexacaftor. The present drug analytes were run at a flow-rate of 0.3ml/ min at 30°C temperature. The injection volume was 2μL and with ultraviolet detection at 270nm. Under these conditions, elexacaftor, ivacaftor and tezacaftor were eluted at 0.72min, 1.4min and 1.9min respectively with a total run time shorter than 5min. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The developed RP-UPLC method was applied successfully for quality control assay of Ivacaftor, Tezacaftor and Elexacaftor in their combination drug product.

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