scholarly journals DEVELOPMENT AND VALIDATION OF METHODS FOR QUANTITATIVE DETERMINATION OF SODIUM HYALURONATE IN THE COMPOSITION OF COMBINED DENTAL GEL

2020 ◽  
Vol 5 ◽  
pp. 72-81
Author(s):  
Dmytro Orlenko ◽  
Volodymyr Yakovenko ◽  
Vyacheslav Plastun ◽  
Liliia Vyshnevska

According to the EP monograph "Sodium hyaluronate" for identification they use the infrared transmission spectrum of the substance, quantification is carried out by spectrophotometry. The aim of the work was to develop a method for quantitative determination of hyaluronic acid in the gel in the presence of other substances and its validation. Materials and Methods. The object of the study were samples of combined dental gel of the following composition: metronidazole benzoate 16 mg/g, miramistin 5 mg / g, sodium hyaluronate 2 mg / g. Identification and quantification of sodium hyaluronate was performed by liquid chromatography (SPhU, 2.2.29, 2.2.46). The test solution and the reference solution were chromatographed, obtaining the number of parallel chromatograms not less than when checking the suitability of the chromatographic system. Chromatography is performed on a liquid chromatograph with a diode-matrix detector under the following conditions: chromatographic column PL-aquagel-OH, Agilent size 300 mm × 7.5 mm, with a particle size of sorbent 8 μm; mobile phase A: 0.1 M sodium sulfate solution; mobile phase B: acetonitrile for chromatography P; detection at a wavelength of 210 nm. Results. The retention time of sodium hyaluronate on the chromatogram of the test sample of the gel coincides with the peak and the retention time on the chromatogram of the comparison solution of the standard sample of the substance. The suitability of the chromatographic system for 3 parallel determinations was checked: the relative standard deviation (RSD) is equal to 0.25, the number of theoretical plates is 980, the symmetry coefficient is 1.293. The validation characteristics of the developed methodology meet the established eligibility criteria. The spectral purity coefficients (Fp) of the sodium hyaluronate peak on the chromatograms of the model solution are Fp1=997.665 and Fp2=997,802. The method is linear in the range of sodium concentration of hyaluronate 80–120 %, the calculated linear dependence of the reduced area of the chromatographic peak on the reduced concentration of sodium hyaluronate is |a|=1.9490≤Δa=2.56. The confidence interval of the unit value for the sample of relations is found / entered Δz=1.08, which corresponds to the condition Δz≤1.6 %. The value of the systematic error is equal to δ=0.12, which satisfies the condition δ≤0.51 %. Conclusions. The method of quantitative determination of sodium hyaluronate by the method of high-performance liquid chromatography has been developed and investigated. The method allows the identification and quantification of sodium hyaluronate in the composition of the dental gel, in the presence of metronidazole benzoate and miramistin. Validation of the methodology was performed and the main validation characteristics were determined. In terms of specificity, linearity, correctness, convergence of the method meets the eligibility criteria established by the SPhU.

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono

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.


2005 ◽  
Vol 88 (4) ◽  
pp. 1020-1027 ◽  
Author(s):  
Monika Strazisar ◽  
Maja Fir ◽  
Alenka Golc-Wondra ◽  
Luka Milivojevic ◽  
Mirko Prosek ◽  
...  

Abstract The dietary sources of CoQ10 and the evaluation of CoQ10 in dairy products were characterized. For quantitation of CoQ10 in food samples, 2 liquid chromatography (LC) methods with UV and mass spectrometry (MS) detections were developed. LC with UV detection was performed at 25°C on a Hyperclone ODS 5 μm 150 × 4.6 mm column with mobile phase consisting of methanol-ethanol-2-propanol (70 + 15 + 15, v/v/v). Flow rate was 1.0 mL/min. Retention time of CoQ10 was 10.9 ± 0.1 min. The method was sensitive [limit of detection (LOD) = 0.2 mg/kg], reproducible [relative standard deviation (RSD) = 3.0%), and linear up to 25 mg/kg (R > 0.999). LC/MS analysis was performed on a LUNA C18 3 μm, 150 × 4.6 mm column, using mobile phase consisting of ethanol-dioxane-acetic acid (9 + 1 + 0.01, v/v/v), flow rate was 0.6 mL/min, and the retention time of CoQ10 was 4.1 ± 0.1 min. Identification and quantitation were performed with a Finnigan-LCQ mass detector in positive atmospheric pressure chemical ionization mode. Mass spectra were obtained in selected-ion monitoring mode; molecular mass (M+H)+m/z 863.4 ± 1 was used for quantitative determination. MS detection is more sensitive than UV detection (LOD = 0.1 mg/kg), less reproducible (RSD = 4.0%), and linear in selected range. Analytical recoveries are 75–90% and depend on the ratio between the amount of fat in the matrix and the concentration of CoQ10 in the sample. Some soybean milk products were analyzed together with different cow, goat, and sheep milk products. Concentrations obtained with LC and LC/MS were compared with a few accessible results available from the literature. Concentrations varied from 0 ppm in soybean milk to nearly 2 ppm in fresh milk from local farms.


Author(s):  
Panchumarthy Ravisankar ◽  
Devala Rao G ◽  
Md Shaheem Sulthana ◽  
Supriya K ◽  
Mounika G ◽  
...  

Objective: Objective of the present investigation is to develop a speedy isocratic reverse phase high-performance liquid chromatography (RP-HPLC) method for the separation and quantitative determination of 5 angiotensin II - receptor antagonists, namely, telmisartan, losartan, valsartan, olmesartan, irbesartan, and atenolol along with thiazide diuretics mostly hydrochlorothiazide (HCTZ).Methods: RP-HPLC method was evolved using Welchrom C18 column (4.6 × 250 mm, 5 μm) as a stationary phase with the mobile phase comprising a variety of phosphate buffer with pH-3.3 and acetonitrile in the proportion of 50:50 v/v. The mobile phase was pumped at a current rate of 1 mL/minute. The detection wavelength was carried out at 230 nm.Results: The total run time was 6 minutes and the elution window of only 3 minutes. The peaks were eluted with decorous resolution. The calibration curves were linear (r2=0.9998) in all cases. The percentage relative standard deviation (RSD%) was <2% and average recovery was above 99.95%. The method was validated specificity, precision, and accuracy. High recovery values and low RSD% prove that this method is very accurate and reproducible. The developed method was applied to the estimation of the above-said drugs in binary combinations from different manufacturers which were a good agreement with label claim.Conclusion: The important advantage of developed method was that the five individual drugs can be determined on a single chromatographic system without alteration in detection wavelength and mobile phase composition. This novel method was statistically validated as per ICH guidelines. The optimized method proved to be linear, accurate, and robust. Hence, the above said proposed method was found to be a rapid tool for the routine determination of the above-said drugs in alone or combination with HCTZ in quality control analysis without interference of excipients.


2017 ◽  
pp. 44-48
Author(s):  
Larisa Sotnikova ◽  
Larisa Sotnikova ◽  
Polina Goryunova ◽  
Polina Goryunova ◽  
Sergey Sozinov ◽  
...  

The present paper illustrates the results of the study on chromatographic behavior and optimization of some parameters of the method of quantitative determination of bornyl acetate and isobornyl acetate diastereomers under the conditions of reversed-phase high- performance liquid chromatography. Chromatography was performed with HPLC platform Agilent 1200 with diode-matrix detector and a column Agilent Zorbax XDB, Extend-C18. Detection of the studied analytes was performed at a wavelength of 210 nm. Determinationof the concentration of bornyl acetate isomers was carried out in mixture with other components of the Abiessibirica essential oil in chromatographic systems with mobile phases of acetonitrile-water or isopropyl alcohol-water. The range of analyte concentrations in a sample was varied from 2 to 430 mg/ml for bornyl acetate and from 2 to 950 mg/ml for isobornyl acetate. It is stated that in a chromatographic system with a mobile phase, based on acetonitrile, the peaks of the studied components have an asymmetric shape, and the retention times of analytes increase with the decrease of their concentrations in a sample. In a chromatographic system with isopropyl alcohol the asymmetry of the bornyl acetate peak disappears, the width decreases and the retention time stabilizes. For isobornyl acetate a peak width also decreases, its asymmetry is preserved, but at the same time, the asymmetry coefficient takes on permitted values (less than 2). Calibration charts for the mentioned compounds in the used eluents are linear throughout the studiedconcentration range with correlation coefficients of R2>0.998. Thus, the conducted researches allow to recommend the reversed-phaseHPLC variant for the separate quantitative determination of bornyl acetate and isobornyl acetate in the pine oil samples.


2018 ◽  
Vol 8 (4) ◽  
pp. 42-47
Author(s):  
Tien Nguyen Huu ◽  
Tram Le Thi Bao ◽  
Ngoc Nguyen Thi Nhu ◽  
Thang Phan Phuoc ◽  
Khan Nguyen Viet

Background: Curcumin is a major ingredient in turmeric (Curcuma longa L., Zingiberaceae), which has important activities such as anti-tumor, anti-inflammatory, antioxidant, anti-ischemia, protection of gastric mucosa etc,. Curcumin can be considered as a biological marker of turmeric and turmeric products. Objectives: Developing an HPLC method for quantification of curcumin in turmeric powder and turmeric - honey ball pills; applying this method for products on the market. Materials and methods: turmeric powder and turmeric - honey ball pills collected in Thua Thien Hue province. After optimization process, the method was validated and applied to evaluate the content of curcumin. Results: The chromatography analysis was performed with: Zorbaz Eclipse XDB-C18 (150 × 4.6 nm; 5 µm); Mobile phase: acetonitril: 2% acetic acid (45:55), Flow rate was kept constant at 1.0 ml/min; Detector PDA (420 nm). The method was validated for the HPLC system compatibility, specificity, linearity range, precision and accuracy; the recovery greater than 98%. Conclusion: The developed HPLC method can determine curcumin in turmeric powder and turmeric - honey ball pills. Key words: Curcumin, turmeric powder, turmeric-honey ball pills, quantitative determination, HPLC


1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


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