Method Development for Leachable Furfural Determination in Wood-Based Panels by HPLC-Uv System

2021 ◽  
Vol 903 ◽  
pp. 223-228
Author(s):  
Daniela Godiņa ◽  
Raimonds Makars ◽  
Rudolfs Berzins ◽  
Aigars Paze ◽  
Janis Rizhikovs

Analytical method has been developed and validated to determine free or leachable furfural concentration in wood-based panels. Particleboards obtained from birch wood and suberinic acids binder were chosen as a reference material. Two methods and two solvents were tested. Acetone extracts of the samples were analyzed with gas chromatography (GC) flame ionization detector system. Water extracts were analyzed with high-performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV) system. After the GC data in acetone extracts furfural concentration was below method limit of detection. HPLC-UV data showed that in water extracts furfural concentration was possible to determine. It was concluded that HPLC-UV is suitable and fast method for furfural determination in wood-based panels water extracts.

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.


2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.


Author(s):  
Sanapala Srinivasa Rao ◽  
A. Vijayalakshmi

Residual solvents in Pharmaceuticals are termed as organic volatile impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical methodology was developed for the quantification of residual solvents in Glipizide using a headspace gas chromatography (HSGC) with the help of flame ionization detector (FID). Methanol, acetone and dimethyl formamide as residual solvents were determined in Glipizide. Analysis was performed by headspace GC/FID method on Auto system- HS40. Nitrogen was used as a carrier gas and the separation of residual solvents was achieved by DB-Wax 0.25mm, 0.3mcm column. The thermostat temperature was 115 °C for 40 minutes for each vial. % RSD for nine injections obtained are in acceptance criteria. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated includes specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. According to the International Conference on Harmonization (ICH) guidelines, a new simple, specific, accurate and precise method was developed and validated.


Author(s):  
HARMITA HARMITA ◽  
HERMAN SURYADI ◽  
LIDWINA DEVIANI LIKASA

Objective: The purpose of this research was to optimize and validate a method for measuring the levels of diallyl disulfide (DADS) and diallyl trisulfide(DATS) in garlic and single clove garlic.Methods: The analysis was performed using gas chromatography (GC) equipped with an HP-1 column and a flame ionization detector. The initialcolumn temperature was set at 140°C and increased at 1°C/min to 180°C. The injector and detector temperatures were set to 200°C, the carrier gasflow rate was 0.80 mL/min, and the injection volume was 1.0 μL. The optimized conditions of analysis were then validated which included selectivity,linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ).Results: Using the validated assay and a concentration range of 0.5–20 μg/mL, the coefficient of correlation (r) for DADS was 0.9999 and the LODand LOQ for DADS were 0.3063 μg/mL and 1.0210 μg/mL, respectively. Using the validated assay and a concentration range of 0.5–20 μg/mL, thecoefficient of correlation for DATS was 0.9999 and the LOD and LOQ for DATS were 0.1986 μg/mL and 0.6621 μg/mL, respectively. The percentage ofrecovery was in the range of 98.05–101.76% and coefficient of variation ≤ 2%.Conclusion: This GC method accurately measures the levels of DADS and DATS in garlic.


Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.


Author(s):  
Sunkara Namratha ◽  
Vijayalakshmi A

Objective: Reversed-phase high-performance liquid chromatographic method (RP-HPLC) was developed for the assessment of lopinavir in the dosage form of tablet.Methods: Chromatogram was run through using Kromosil C18 4.5×150 mm using a mobile phase methanol: water of ratio 65:35% v/v with a rate of flow of 0.8 ml/min, measured by UV spectrometric detection at 265 nm. The method developed was validated in terms of precision, accuracy, linearity, and robustness parameters.Results: Retention time of lopinavir established at 2.482 min and percentage R.S.D of lopinavir found to be 1.0% and 0.5%, respectively. The method shows that good linearity range of 30–150 μg correlation coefficient of lopinavir was 0.997. The limit of detection was 2.97 and limit of quantification was 9.92, respectively. The percent purity of lopinavir was 99.87%.Conclusion: The suggested method (Rp-HPLC) for concurrent assay lopinavir was validated, which is appropriate method for the analysis oflopinavir quantitatively in tablet dosage forms and bulk.


2014 ◽  
Vol 4 (1) ◽  
pp. 51 ◽  
Author(s):  
Vania Maria Moreira Valente ◽  
Gulab Newandram Jham ◽  
Carolina Marangon Jardim ◽  
Onkar Dev Dhingra ◽  
Ion Ghiviriga

<p>Aiming to substitute toxic synthetic fungicides, the activity of nutmeg (<em>Myristica fragrans</em>) essential oil (EO, obtained by hydrodistillation) was investigated against two important storage fungi-<em>Aspergillus flavus</em> <em>A. ochraceus</em>. The activity of crude nutmeg EO was investigated using poison food assay (PFA). At a concentration of 0.1%, the EO inhibited <em>A. flavus</em> and <em>A. ochraceus</em> growth by 43 and 65%, respectively. At a concentration of 0.3 %, <em>A. flavus</em> and <em>A. ochraceus</em> inhibitions were 84 and 79%, respectively. The crude nutmeg EO on fractionation by preparative TLC-bioautography presented one band from which two pure compounds were isolated by semi-preparative normal-phase high performance liquid chromatography. Myristicin and safrole were identified by nuclear magnetic resonance (<sup>1</sup>H and <sup>13</sup>C) and gas chromatography-mass spectrometry. The relative % of myristicin and safrol in the crude EO was 10.8 and 2.9, respectively, determined by gas chromatography with a flame ionization detector. The crude EO, the isolated active fraction, isolated myristicin and standard myristicin presented similar activities against the two fungi at concentrations of 0.1 and 0.3% by PFA. Based on these results it is concluded that myristicin is the major antifungal in nutmeg EO against <em>A. flavus</em> and <em>A. ochraceus</em>.</p>


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