scholarly journals EXTRACTION, CLEAN-UP, AND HPLC DETECTION OF CARBARYL AND CARBOFURAN FROM CABBAGE (Brassica oleracea)

2010 ◽  
Vol 9 (3) ◽  
pp. 452-456 ◽  
Author(s):  
Iip Izul Falah
Keyword(s):  
Brassica Oleracea ◽  
Mobile Phase ◽  
Harmful Effect ◽  
Liquid Extraction ◽  
Good Separation ◽  
Carbamate Pesticides ◽  
Liquid Liquid Extraction ◽  
Better Than

Carbaryl (1-naphthyl-N-methylcarbamate) and carbofuran (2,3-dihydro-2,2-dimethyl-7-benzofuranol-N-methylcarbamate) are very important N-methylcarbamate pesticides due to their high insecticide and nematocide effects, and widely used in vegetables plantations. The increasing use of carbamate pesticides poses a risk to human and environment. Thus, it is necessary to quantify their residue amount in food and vegetables to prevent harmful effect on animals, human and environment. This work was aimed to study of carbaryl and carbofuran analysis from fortified cabbage (Brassica oleracea) by liquid-liquid extraction, clean-up using SPE, followed by HPLC detection. Result of the work showed that detection of carbaryl using spectrophotometer detector at wavelength of 220 nm was better than at 230 and 280 nm, respectively. When the carbamates were extracted from cabbage using methanol, followed by liquid-liquid extraction using dichloromethane, cleaned-up with SPE-C18 and eluted by acetonitrile, the recovery was 96.8%. The detection by HPLC involved 4.6 x 25 mm, 5 µm C18 column, spectrophotometer detector at wavelength of 220 nm, and isocratic mobile phase at ratio of 35:65 of acetonitrile:aquabidest gave a good separation between co-extracted compounds and the carbamates.   Keywords: HPLC, carbaryl, carbofuran, extraction, clean-up

scholarly journals RP-HPLC Method Development and Its Validation for Quantitative Determination of Rimonabant in Human Plasma

2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Shravan Bankey ◽  
Ganesh Tapadiya ◽  
Jasvant Lamale ◽  
Deepti Jain ◽  
Shweta Saboo ◽  
...  
Keyword(s):  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Bioequivalence Study ◽  
Hplc Method ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Hplc Method Development

A simple, accurate, and precise HPLC method was developed and validated for determination of rimonabant in human plasma. Following liquid-liquid extraction, chromatographic separation was accomplished using C18 column with mobile phase consisting of acetonitrile : water (90 : 10, v/v), drug was detected at 260 nm using UVdetector. The LOD and LOQ were 3.0 and 10.0 μg/L, respectively. The method is linear in the interval 50.0–1000.0 μg/L. The average extraction recovery of drug from plasma was found to be 92.2%. The percent CV of the method was found to be less than 10.8%, and accuracy was found between 94.5 and 106.7%. The assay may be applied to a pharmacokinetic and bioequivalence study of rimonabant.

scholarly journals Retinol, cholecalciferol and alpha-tocopherol contents of Bulgarian Black Sea fish species

2012 ◽  
Vol 23 (1) ◽  
pp. 31-34
Author(s):  
Mona Stancheva ◽  
Diana A. Dobreva ◽  
Bistra Galunska
Keyword(s):  
Black Sea ◽  
Mobile Phase ◽  
Tocopherol Content ◽  
Liquid Extraction ◽  
Alpha Tocopherol ◽  
Liquid Liquid Extraction ◽  
Sample Preparation Procedure ◽  
Psetta Maxima ◽  
Sea Fish ◽  
Belone Belone

AbstractThe aim of the present study is to determine and to compare the content of retinol, cholecalciferol and alpha-tocopherol in edible tissue of two Black sea fishes - Garfish (Belone belone) and Turbot (Psetta maxima). All-trans-retinol (vitamin A), cholecalciferol (vitamin D3) and alpha-tocopherol (vitamin E) were analyzed simultaneously using HPLC/UV/FL system (Thermo Scientific Spectra SYSTEM) equipped with RP analytical column. The mobile phase was composed of 97:3 = MeOH:H2O. Retinol and cholecalciferol were monitored by UV detection at lmax = 325 nm and lmax = 265 nm, respectively. Alpha-tocopherol was detected by fluorescence at lex=288 nm and lem=332 nm. The sample preparation procedure includes alkaline saponification, followed by liquid-liquid extraction. Quantities of all-trans-retinol and cholecalciferol were higher in garfish tissues while alpha-tocopherol content in turbot showed seven times higher values.

scholarly journals Development of a UHPLC-MS/MS method for the determination of quercetin in milk and its application to a pharmacokinetic study

2019 ◽  
Vol 63 (1) ◽  
pp. 87-91
Author(s):  
Małgorzata Gbylik-Sikorska ◽  
Anna Gajda ◽  
Artur Burmańczuk ◽  
Tomasz Grabowski ◽  
Andrzej Posyniak
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Therapeutic Agent ◽  
Clinical Mastitis ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Repeatability And Reproducibility ◽  
The Mean

Abstract Introduction: Quercetin is a polyphenolic flavonoid which has been used in traditional Chinese medicine as a natural therapeutic agent with a broad spectrum of activities (antioxidant, anticancer, neuroprotective, anti-inflammatory, antiviral and antibacterial). The aim of this study was to develop and validate a rapid and simple ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) method for the determination of quercetin in milk. Material and Methods: Sample preparation was based on a liquid-liquid extraction with 0.5% formic acid in acetonitrile. The chromatographic separation was performed on a ZORBAX SB-C18 column with methanol and 0.5% formic acid as a mobile phase. Results: The procedure was successfully validated. The mean recovery of the analyte was 98%, with the corresponding intra- and inter-day variation less than 10% and 15%, respectively, and the repeatability and reproducibility were in the range of 3%–7.2% and 6.1%–12%, respectively. The lowest level of quantification was 1.0 μg/kg. Conclusion: The proposed method was successfully applied in evaluating the pharmacokinetics of quercetin in milk obtained from dairy cows with clinical mastitis after intramammary administration.

Acetonitrile as tops solvent for liquid chromatography and extraction

2018 ◽  
Vol 1 (2) ◽  
Author(s):  
Oleg Borisovich Rudakov ◽  
Liudmila V. Rudakova ◽  
Vladimir F. Selemenev
Keyword(s):  
Mobile Phase ◽  
Chemical Properties ◽  
Refraction Index ◽  
Extraction Methods ◽  
Reversed Phase ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Optic Density ◽  
Mobile Phases ◽  
Physico Chemical

This article deals with acetonitrile physico-chemical properties and its mixtures with water. It covers the information about isotherms of such parameters of the acetonitrile-water binary system as density, viscosity, permeation coefficient, refraction index, optic density, a boiling point isobar. Authors suggest a generalized criterion of acetonitrile polarity. The article also discusses means of polarity assessment and eluotropic strength of mobile phases on the basis of acetonitrile mixtures with water with application of generalized criteria. Special attention is paid to the options of acetonitrile application in various extraction methods of chromatographic sample preparation. The article also reveals advantages and problems of acetonitrile application as a mobile phase modifying agent in the HPLC reversed-phase and as a hydrophilic extra-agent in liquid-liquid extraction.

scholarly journals SYNTHESIS AND STORAGE OF SINGLE PHENYLTIN COMPOUNDS SYNTHESIZED FROM ISOTOPICALLY ENRICHED TIN METAL

2009 ◽  
Vol 12 (17) ◽  
pp. 42-54
Author(s):  
Van Nguyen Dong ◽  
Wolfgang Frech ◽  
Solomon Tesfalidet
Keyword(s):  
Acetic Acid ◽  
Ionic Strength ◽  
Aqueous Phase ◽  
Sodium Acetate ◽  
Single Species ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Tin Metal ◽  
And Storage ◽  
Better Than

A method combining liquid liquid extraction and chromatographic fractionation has been developed for the preparation of pure monophenyltin (MPT), diphenyltin (DPhT), and triphenyltin (TPhT), synthesized from isotope enriched Sn-metal using phenylation of SnI4 in diethylether (DEE) followed by quenching with HBr and water. After two successive extractions of the aqueous HBr phase with DEE, more than 99% of the DPT and TPhT were recovered in the combined DEE phase and 94% of the MPT remained in the aqueous phase. The MPT in the aqueous phase was extracted into dichloromethane. The organic phases were vaporised and the PhTs were re-dissolved in MeOH/water/acetic acid/sodium acetate (59/30/6/8, v/v/v/w), which was also used as storing solution. Aliquots of the two solutions containing either DPhT and TPhT or MPhT were injected into a silica based C18 column for isolating and purifying single species. The yield of the purification of MPhT, DPT, and TPht was better than 99%. At -20 °C, all the fractionated phenyltin species were stable in the storing solution for at least 197 days. When these standards were stored at 4 °C or 22°C, 4% to 6% of DPhT and TPhT degraded during 27 days. The degradation of DPT and TPht increased with the ionic strength and acidity of the storage solution.

scholarly journals A VALIDATED LC-MS/MS METHOD FOR PHARMACOKINETIC STUDY OF CANAGLIFLOZIN IN HEALTHY RABBITS

2018 ◽  
Vol 10 (2) ◽  
pp. 80 ◽  
Author(s):  
Darshan Bhatt ◽  
B. Rajkamal
Keyword(s):  
Pharmacokinetic Study ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Liquid Extraction ◽  
Tandem Mass ◽  
Rabbit Plasma ◽  
Liquid Liquid Extraction ◽  
Test Formulation ◽  
Liquid Chromatography Tandem Mass ◽  
The Mean

Objective: A liquid chromatography-tandem mass spectrophotometric (LC-MS/MS) method was developed for quantification of canagliflozin in rabbit plasma employing Liquid-Liquid extraction technique.Methods: Chromatographic separation was achieved on Inertsil ODS 5 µm C18, 50×4.60 mm with 30:70 v/v of 0.01M ammonium acetate: methanol as an isocratic mobile phase with a flow rate of 0.8 ml/min. The developed LC-MS method was applied to assess Cmax, t1/2, AUC0-t, and AUC0-inf of canagliflozin tablet after oral administration in healthy rabbits.Results: The developed method was linear over working range of 5ng/ml to 600ng/ml with a coefficient of correction (r2) = 0.999. The % recovery of the method was found to be 102.05%. The mean intraday and inter-day precision of the method was found to be 0.77 to 3.72%. The Canagliflozin showed Tmax of 1.58±0.2 and mean Cmax, AUC0®t andAUC0®a for Test formulation is 272±13.24, 2571.20±251and 2777.43±276 respectively.Conclusion: The developed method can be applied for routine analysis for quality control and the established LLOQ is sufficiently low to conduct a pharmacokinetic study with any marketing formulation of Canagliflozin in healthy rabbits.

scholarly journals Aktivitas Antidiare Daun Harendong (Malestoma malabathricum L)

2020 ◽  
Vol 2 (1) ◽  
pp. 39-48
Author(s):  
Ika Kurnia Sukmawati ◽  
Elin Yulinah Sukandar ◽  
Neng Fisheri Kurniati
Keyword(s):  
Antibacterial Activity ◽  
Castor Oil ◽  
Leaf Extract ◽  
Shigella Flexneri ◽  
Extraction Methods ◽  
Salmonella Typhi ◽  
Liquid Extraction ◽  
Shigella Dysenteriae ◽  
Liquid Liquid Extraction ◽  
Better Than

Diarrhea still become main health problem especially in several developing countries including Indonesia. Hharendong leaf have been used by people traditionally as the treatment of various Gastrointestinal tract disorders including diarrhea. The purpose of this study was tested antidiarrhea and antibacterial activity of extracts and fractions of the three selected plants. The extraction was conducted using reflux method with ethanol 96% as solvent. Extract was fractinated by liquid-liquid extraction methods using n-hexane and ethylacetate solvents gradually. Antimicrobial activity assays was performed by using broth microdiluiton methods toward extract and fractions of plants selected. Escherichia coli, Shigella dysenteriae, Shigella flexneri, and Salmonella typhi. were used as microbes test. Antidiarhhea activity was tested to diarrhea animal induced by castor oil. Dosage test was given one hour before induction then carried out observations of feces (frequency, consistency and weight). Transit intestinal method was also performed in this experiment with comparing the length of the intestinal through by marker with the total length of the intestine. Antidiarrhea activity result have shown that Harendong leaf extract at the doses 50 and 100 mg/kg BW showed decreased of frequency ,consistency and weight of feces better than another extract. Ethylacetate fraction of the leaf harendong showed antibacterial activity to Shigella dysenteriae ( MIC of 128 µg/ml), dan Salmonella typhi (MIC 512 µg/ml), and fraction n-heksan of the leaf harendong showed antibacterial activity to Shigella dysenteriae and Salmonella typhi the MIC 512 µg/ml.

scholarly journals DETERMINATION OF CARBAMATE RESIDUES IN VEGATABLES, BULBS AND WATER

2020 ◽  
Vol 12 (9) ◽  
pp. 78-87
Author(s):  
Liem Van Nguyen ◽  
Dong Van Nguyen ◽  
Hien Thi To
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Liquid Extraction ◽  
Fluorescent Compound ◽  
Phase Gradient ◽  
Liquid Liquid Extraction ◽  
Limit Of Quantitation

A method for the determination of residues of 10 carbamates including Aldicard Sulfoxide, Aldicarb sulfone, Oxamyl, Methomyl, 3-Hydroxycarbofuran, Aldicarb; Propoxur, Carbofuran, Carbaryl and Methiocarb in vegetables, bulbs and water was established based on High Performance Liquid Chromatography with fluorescence detection after derived post column. Solid samples were grinded in MeOH, clarify. Extraction liquid or water samples were cleaned by liquid-liquid extraction or SPE C18 Carbamates were extracted in HPLC C18 with mobile phase gradient MeOH/H2O and derived phthalaldehyde (OPA) and 2 - mercaptoethanol. A fluorescent compound 1 - hydroxytylthio - 2-metylisoindol was produced and detected by fluorescence detection with λex 340 nm and λem 445 nm. Limit of detection and limit of quantitation for the carbamates were 0.51 - 5.0 ppb and 1.69-9.09 ppb, respectively. The recoveries of the carbamates were from 73 to 95%. The concentrations of the carbamate in vegetables, bulbs and water at some investigated sites were low.

scholarly journals A VALIDATED LC-MS/MS METHOD FOR PHARMACOKINETIC STUDY OF BRIVARACETAM IN HEALTHY RABBITS

2018 ◽  
Vol 10 (2) ◽  
pp. 24
Author(s):  
D. Atul Vasanth ◽  
B. Rajkamal
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Multiple Dose ◽  
Liquid Extraction ◽  
Pharmacokinetic Studies ◽  
Tandem Mass ◽  
Liquid Liquid Extraction ◽  
Test Formulation ◽  
Liquid Chromatography Tandem Mass ◽  
The Mean

Objective: A liquid chromatography-tandem mass spectrophotometric (LC–MS/MS) method was developed for quantification of brivaracetam in rabit plasma employing liquid-liquid extraction with ethyl acetate.Methods: Developed method was validated for specificity, precision, accuracy, recovery, and stability characteristics. Chromatographic separation was achieved on Chromolith C18column (100 mmx4.6 mmx5 µm) with 0.1% formic acid, adjusted to pH 3.2 as an isocratic mobile phase with a flow rate of 1.0 ml/min. the developed method was applied to assess pharmacokinetics parameters like Cmax, Tmax, t1/2 and AUC of brivaracetam in healthy rabbits.Results: The developed method was linear over the range of 0.16 to 8µg/ml. The regression equation for the analysis was Y=0.0053x+0.0018 with coefficient of correction (r2) = 0.998. The % mean recovery for brivaracetam was found to be between 95.7% to 106.5%. The mean intraday and inter-day precision of the method was found to be 0.77 to 3.72% for quality control standards. Brivaracetam showed Tmax of 1.025±0.061 and mean Cmax, AUC0®t andAUC0®a for Test formulation is 92.7±4.4, 496.21±26.4 and 504.20±30.68 respectively.Conclusion: A highly specific, rugged and rapid method with sufficiently low LLOQ was developed for analysis of routine samples of a single dose or multiple dose pharmacokinetic studies with any marketing formulation of brivaracetam.

scholarly journals Selective Liquid Chromatographic Method for Determination of Fluoxetine in Plasma

2001 ◽  
Vol 84 (6) ◽  
pp. 1735-1738 ◽  
Author(s):  
Afshin Zarghi ◽  
Abbas Kebriaeezadeh ◽  
Reza Ahmadkhaniha ◽  
Maryam Akhgari ◽  
Nooshin Rastkari
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Antidepressant Drugs ◽  
Liquid Extraction ◽  
Tricyclic Antidepressant ◽  
Liquid Liquid Extraction ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract A selective and sensitive liquid chromatographic method was developed for the determination of fluoxetine (FLU) in plasma. FLU was isolated from plasma by liquid–liquid extraction. The chromatographic separation was performed on an analytical 250 × 3.9 mm id Novapak C18 column (4 μm particle size) with an isocratic mobile phase consisting of phosphate buffer–acetonitrile–methanol–triethylamine (58 + 30 + 10 + 2, v/v) adjusted to pH 7. Using UV detection at 226 nm, the detection limit for FLU in plasma was 3 ng/mL. No interferences were found with tricyclic antidepressant drugs, which allows this method to be used in clinical studies. The calibration curve was linear over the concentration range of 10–200 ng/mL. The average recovery was about 80% for plasma. The inter- and intraday assay coefficients of variation were <8%.

Sign in / Sign up

Export Citation Format

Share Document