Validated Stability-Indicating Methods for the Simultaneous Determination of Amiloride Hydrochloride, Atenolol, and Chlorthalidone Using HPTLC and HPLC with Photodiode Array Detector

2013 ◽  
Vol 96 (2) ◽  
pp. 313-323 ◽  
Author(s):  
Rasha M Youssef ◽  
Hadir M Maher ◽  
Eman I El-Kimary ◽  
Ekram M Hassan ◽  
Magda H Barary
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Pharmaceutical Preparations ◽  
Array Detector ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Chromatographic Methods ◽  
Photodiode Array ◽  
Amiloride Hydrochloride

Abstract Two stability-indicating chromatographic methods are described for simultaneous determination of amiloride hydrochloride (AMI), atenolol (ATE), and chlorthalidone (CHL) in combined dosage forms. The first method was based on HPTLC separation of the three drugs followed by densitometric measurements of their bands at 274 nm. The separation was carried out on Merck HPTLC silica gel 60F254 aluminum sheets using chloroform–methanol–ammonia 27%, w/w (9 + 2 + 0.3, v/v/v) mobile phase. Analysis data was used for the linear regression graph in the range of 0.1–0.5, 0.8–5.0, and 0.3–1.5 μg/band for AMI, ATE, and CHL, respectively. The second method was based on an RP-HPLC separation of the cited drugs performed on an RP stainless steel C18 analytical column (250 × 4.6 mm id) with a gradient elution system of methanol and 0.05 M aqueous phosphate buffer adjusted to pH 4 as the mobile phase, at the flow rate of 1.0 mL/min. Quantitation was achieved with photodiode array detection at 275 nm for AMI and 225 nm for ATE and CHL. The calibration graphs for each drug were rectilinear in the range of 2–50, 25–150, and 2–100 μg/mL for AMI, ATE, and CHL, respectively. The proposed chromatographic methods were successfully applied for determination of the investigated drugs in pharmaceutical preparations. Both methods were validated in compliance with International Conference on Harmonization guidelines in terms of linearity, accuracy, precision, robustness, LOD, and LOQ.

scholarly journals A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Ali S. Abdelhameed ◽  
Samar A. Afifi
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Rat Plasma ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Interday Precision

A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear withr2=0.9999for PTZ andr2=0.9995for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH) guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD) <7.76% for PTZ and <7.58 % for ETD.

Stability Indicating Photodiode Array Detector Based Estimation of Dapagliflozin Propanediol Monohydrate in API and Tablet Dosage Form by RP-UPLC

2021 ◽  
pp. 4635-4639
Author(s):  
Ashok B. Patel ◽  
Ekta H. Vaghasiya ◽  
Amit R. Dudhatra ◽  
Amitkumar J. Vyas ◽  
Ajay I. Patel ◽  
...  
Keyword(s):  
Dosage Form ◽  
Active Pharmaceutical Ingredient ◽  
Array Detector ◽  
Column Temperature ◽  
Stability Indicating ◽  
Photodiode Array Detector ◽  
Acceptable Method ◽  
Photodiode Array ◽  
Tablet Dosage

Stability indicating RP-UPLC photo diode array detector based method for determination of Dapagliflozin propanediol monohydrate (DPM) in active pharmaceutical ingredient (API) and in tablet dosage form (5mg dapagliflozin) has been developed and validated on Bridge Ethylene Hybride (BEH) C18 column (50mm × 2.1 mm, 1.7µm). Mobile phase composition was water: acetonitrile (60:40 v/v), flow rate 0.5ml/min and detection carried out at 223nm at column temperature 30ºC. Chromatographic separation achieved within 2 min with retention time 0.77 min. Linearity of the method was found over the concentration range of 25-75µg/ml (R2 = 0.9977). The degradation was carried out in five different stress conditions. The developed method was able to resolve peak of API from all generated peaks. Sufficient degradation was achieved in the range of 5.25 to 12.31%. The peak purity is acceptable, Method validation was performed as per ICH guideline Q2(R1).

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

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 &lt;1 and &lt;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 &gt;2 from the nearest peak. Insignificant changes in retention time (&lt;4) and calculated amount (&lt;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 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.

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