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

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.

2017 ◽  
Vol 15 (1) ◽  
pp. 293-298
Author(s):  
Pakinaz Y. Khashaba ◽  
Hassan Refat H. Ali ◽  
Mohamed M. El-Wekil

AbstractA simple, rapid, cost-effective, and sensitive TLC-spectrodensitometric method for simultaneous determination of esomeprazole and domperidone was developed and tested in human plasma. Ethyl acetate: methanol: benzene: acetonitrile (5: 4: 8: 3, v/v/v/v) mobile phase was used for separation on TLC plates detected at 286 nm. The linearity ranges were 5-1200 and 2-600 ng/ spot for esomeprazole and domperidone, and limits of detection were 1.73 and 0.59 ng/spot. The effects of four variables affecting Rf were evaluated by fractional factorial design. The benzene volume and saturation time had significant effects.


2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal

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.


2010 ◽  
Vol 93 (4) ◽  
pp. 1086-1092 ◽  
Author(s):  
Anna Gumieniczek ◽  
Anna Berecka ◽  
ukasz Komsta

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.


1995 ◽  
Vol 78 (4) ◽  
pp. 1067-1071 ◽  
Author(s):  
David C Holland ◽  
Robert K Munns ◽  
José E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long

Abstract A liquid chromatographic (LC) method is described for the simultaneous determination of the triazine herbicides, simazine (SIM), atrazine (ATZ), and propazine (PRO) in the 12.5–100 ppb range in catfish. The herbicides are extracted from catfish homogenates with ethyl acetate, followed by solvent partitioning between acetonitrile and petroleum ether and additional cleanup on a C18 cartridge. A Supelcosil LC-18-DB column is used for LC separation, and UV determination is at 220 nm. The isocratic mobile phase is a mixture of methanol, acetonitrile, and water. Mean recoveries from catfish were 88.7, 96.9, and 91.7%; standard deviations were 6.84,7.78, and 6.26%; and coefficients of variation were 7.72,8.03, and 6.82% for SIM, ATZ, and PRO, respectively.


2021 ◽  
Vol 25 (12) ◽  
pp. 107-115
Author(s):  
V.V.S.S.N. Raju Sri Datla ◽  
Manikandan Ayyar

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.


2001 ◽  
Vol 84 (3) ◽  
pp. 684-688 ◽  
Author(s):  
Pei-Lan Wang ◽  
Liang Chen ◽  
Ying-Fang Fan

Abstract This paper reports the determination of trace levels of 5 types of fluorinated quinolone drugs, i.e., ciprofloxacin, norfloxacin, enoxacin, pefloxacin, and ofloxacin, by thin-layer chromatography (TLC)/fluorescence densitometry. The new analytical method uses 2-step TLC development, selective separation, and simultaneous determination of the 5 drugs. The method was also applied to the determination of recoveries of standards of the 5 drugs in plasma and urine samples. The results show that the method has a wide linear range, high repeatability, and good stability.


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

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.


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