Development and validation of a LC-UV Method Applied to the Quality Control of Ursodeoxycholic Acid in Raw Material and Pharmaceutical Formulations

Boscolo, Oriana; Flor, Sabrina; Dobrecky, Cecilia; Salvo, Leandro; Trípodi, Valeria; Lucangioli, Silvia

doi:10.9790/3013-070201111116

Cited by 5 publications

(8 citation statements)

References 7 publications

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“…23 The linearity results obtained the correlation coefficient (R) for the assay and dissolution test of 1 and 0.9995, respectively. The linearity results in this study show in a fairly good R value than previous studies for assay that resulted (R) 0.9951 24 , and (R) 0.9998 25 . Whereas for the dissolution test from previous study the (R) value was (R) 0.9990.…”

Section: Discussionsupporting

confidence: 54%

“…From the LOD and LOQ values in present study, this method still satisfy for quantification of Ursodeoxycholic acid in formulation because from previous research the usual concentration of Ursodoxycholic acid from sample formulation in the test solution in between 200-15000 µg/mL. 7,9,10,11,14,23,24,25,26,27 From the results assay of Ursodeoxycholic acid capsule samples, it was obtained the average concentration of 6 capsules was 103.50±1.47% and Ursodeoxycholic acid dissolved was 97.61±3.97%. This value meets the requirements set by the USP 42 nd for assay between 90-110% and dissolution test ≥ 80%…”

Section: Discussionmentioning

confidence: 64%

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Analytical Method Development of Content and Dissolution Assay of Ursodeoxycholic Acid Capsule

Megawati

Damayanti

2021

IJPST

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Ursodeoxycholic acid is an active compound to treat cholesterol gallstones and included in Biopharmaceutical Classification System class II. Ursodeoxycholic acid capsule formulations have been developed by the pharmaceutical industries. Due to requirement, assay and dissolution tests need to be routinely carried out to control quality of the drug. Therefore, aim of this study was to develop a simultaneously analytical method for assay and dissolution test. Optimum condition of analysis were using HPLC-RID, C 18 column (5 µm; 3.9 x 300 mm), acetonitrile:phosphate buffer pH 3.0 (55:45 v/v) as mobile phase with flow rate 1 mL/min, 50 µL injection volume, column, detector, and sample temperature were set at 40 o C. This method provides good linearity in a range of 50-130 % concentration for assay and dissolution test with correlation coefficient values of 1 and 0.999. respectively. LOD and LOQ for assay were of 4.892 µg/mL and 14.824 µg/mL whereas for dissolution tests of 6.501 µg/mL and 19.701 µg/mL. The average percent recovery for assay and dissolution test were in a range of 100.018±0.888% and 98.936±2.124 %. Repeatability and intermediate precision of assay were obtained by determining RSD values of 0.466% and 0.279-0.483 %, while the dissolution test were 1.137% and 0.032-0.289 %.

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Section: Discussionsupporting

confidence: 54%

Section: Discussionmentioning

confidence: 64%

Analytical Method Development of Content and Dissolution Assay of Ursodeoxycholic Acid Capsule

Megawati

Damayanti

2021

IJPST

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“…UDCA concentration was determined by HPLC-UV [ 41 ]. HPLC was equipped with a reverse phase C18 column—Waters Symmetry (150 mm × 4.6 mm, id; 5 μm particle size).…”

Section: Methodsmentioning

confidence: 99%

“…Therefore, it met the USP specification for dissolution testing. The UDCA content was determined by HPLC-UV according to a previous work [41]. In this sense, the official USP UDCA monograph describes a liquid chromatography (LC) method coupled to a differential refractive index detector due to the low absorptivity of bile acids.…”

Section: Dissolution Testmentioning

confidence: 99%

Formulation and Characterization of Ursodeoxycholic Acid Nanosuspension Based on Bottom-Up Technology and Box–Behnken Design Optimization

Boscolo,

Flor,

Salvo

et al. 2023

Pharmaceutics

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Background: Ursodeoxycholic acid (UDCA) is a therapeutic agent used for the treatment of cholestatic hepatobiliary diseases in pediatric patients. It is a bile acid that presents high lipophilicity, and it belongs to Class II of the Biopharmaceutical Classification System (BCS), which exhibits low water solubility and high intestinal permeability, which leads to poor oral absorption. The objective of this work was to design and optimize UDCA nanosuspensions by means of the precipitation-ultrasonication method to improve the solubility, dissolution, and oral bioavailability of UDCA. Methods: A three-level, three-factor Box–Behnken design was used to optimize formulation variables and obtain uniform, small-particle-size UDCA nanosuspensions. The independent variables were: stabilizer percentage (X1), amplitude (X2), and sonication time (X3), and the dependent variable was the particle size (Y1). In the precipitation–ultrasonication method, UDCA was dissolved in acetone:PEG 400 (1:1 v/v) and quickly incorporated into the antisolvent (pre-cooled aqueous dispersion of HPMC E-15 0.3%), by means of intense sonication at 50 W for 5 min, controlling temperature through an ice water bath. The lyophilization efficacy was evaluated by means of a cryoprotective efficacy test, working with 10% maltose at −80 °C. The nanosuspensions were characterized by dynamic light scattering (DLS), X-ray diffraction, and scanning electron microscopy (SEM). The physicochemical stability was determined at 25 °C and 4 °C at 7, 14, 30, and 60 days, and the UDCA content was analyzed via HPLC-UV. An in vitro dissolution assay and an oral bioavailability study were performed in male Wistar rats. Results: A significant impact was achieved in the optimized nanosuspension with 0.3% (stabilizer), 50 W (amplitude), and 5 min (sonication time), with a particle size of 352.4 nm, PDI of 0.11, and zeta potential of −4.30 mV. It presented adequate physicochemical stability throughout the study and the UDCA content was between 90% and 110%. In total, 86% of UDCA was dissolved in the in vitro dissolution test. The relative oral bioavailability was similar without significant statistical differences when comparing the lyophilized nanosuspension and the commercial tablet, the latter presenting a more erratic behavior. The pharmacokinetic parameters of the nanosuspension and the commercial tablet were Tmax (1.0 ± 0.9 h vs. 2.0 ± 0.8 h, respectively), Cmax (0.558 ± 0.118 vs. 0.366 ± 0.113 µM, respectively), ΔCmax (0.309 ± 0.099 vs. 0.232 ± 0.056, respectively), AUC (4.326 ± 0.471 vs. 2.188 ± 0.353 µg/mL.h, respectively, p < 0.02), and IAUC0–24h (2.261 ± 0.187 µg/mL.h vs. 1.924 ± 0.440 µg/mL.h, respectively). Conclusions: The developed nanosuspension presents an appropriate dosage and administration for pediatric patients. On the other hand, it exhibits an adequate absorption and UDCA oral bioavailability.

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“…To determine the assay of the drug during the storage period, stability indicating analytical method play an important role. There are few analytical methods developed by HPLC for the estimation of ursodeoxycholic acid in ursodeoxycholic acid tablets and capsules [9][10][11][12][13]. From the literature survey, it was observed that there is no stability indicating analytical method available for determination of drug quantity during stability studies.…”

Section: Introductionmentioning

confidence: 99%

Chromatographic Method Development and Validation for Quantitative Determination of Ursodeoxycholic Acid in Ursodeoxycholic Acid Tablets

Sawant¹,

Mane²

2018

Asian J. Chem.

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An HPLC assay method is developed for quantitative determination of ursodeoxycholic acid in ursodeoxycholic acid tablets. The developed method is a simple, accurate, rugged, precise and stability indicating chromatographic method. The stationary phase used in separation of known impurities and ursodeoxycholic acid drug was C18, 250 mm × 4.6 mm, 5 µm. The mobile phase was prepared by mixing of buffer and acetonitrile in the ratio of 50:50 v/v pumped at a flow rate of 1.5mL/min. The developed chromatographic method is validated. The method is accurate, precise and linear over the concentration range of 50-150 %. Mean recovery of ursodeoxycholic acid tablets is found 99.7 ± 0.4. The method is simple and stability indicating, and hence can be used by common laboratories for the determination of ursodeoxycholic acid (assay) in ursodeoxycholic acid ER tablets.

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Development and validation of a LC-UV Method Applied to the Quality Control of Ursodeoxycholic Acid in Raw Material and Pharmaceutical Formulations

Cited by 5 publications

References 7 publications

Analytical Method Development of Content and Dissolution Assay of Ursodeoxycholic Acid Capsule

Analytical Method Development of Content and Dissolution Assay of Ursodeoxycholic Acid Capsule

Formulation and Characterization of Ursodeoxycholic Acid Nanosuspension Based on Bottom-Up Technology and Box–Behnken Design Optimization

Chromatographic Method Development and Validation for Quantitative Determination of Ursodeoxycholic Acid in Ursodeoxycholic Acid Tablets

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