Quantitative determination of fullerene (C60) in soils by high performance liquid chromatography and accelerated solvent extraction technique

2010 ◽  
Vol 7 (3) ◽  
pp. 292 ◽  
Author(s):  
Ali Shareef ◽  
Guihua Li ◽  
Rai S. Kookana
Keyword(s):  
Solvent Extraction ◽  
Quantitative Determination ◽  
Analytical Methods ◽  
Environmental Fate ◽  
Accelerated Solvent Extraction ◽  
Soil Matrix ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Terrestrial Environments

Environmental context.Due to the increasing adoption of nanotechnology, synthetic nanoparticles such as fullerenes (nC60), are likely to emerge as contaminants in aquatic and terrestrial environments. Currently, our understanding of the fate and effects of C60 in the terrestrial environment is poor and is primarily hampered by the lack of reliable quantitative analytical methods. In this paper, we describe a method for effective extraction and sensitive detection of C60 residues in soils which will facilitate environmental fate studies on nC60. Abstract.Fullerenes (e.g. C60) are emerging as environmental contaminants due to their wide range of applications, such as in optics, electronics, cosmetics and biomedicine. Residue analysis is a crucial step in understanding the fate and effects of C60 in the terrestrial environments. However, there is a lack of reliable quantitative analytical methods for extraction and analysis of C60 in soils or sediments. We developed a method for determination of C60 in soils using accelerated solvent extraction (ASE) followed by HPLC-UV detection. Separation of C60 from soil matrix interferences was achieved by gradient elution using methanol–toluene mobile phase. Mean recoveries obtained from extraction efficiency tests using six contrasting soils spiked (wet and dry tests with freeze drying of wet and aged soils before ASE) at varying concentrations of C60 ranged from 84 to 107%. The current method provides adequate sensitivity (limit of quantitation = 20 μg kg–1), and can be used for quantitative determination of C60 in soils and sediments (especially for environmental fate studies) without needing expensive HPLC-mass spectrometry.

DETERMINATION OF PAHs IN WASTEWATER IRRIGATED AGRICULTURAL SOIL USING ACCELERATED SOLVENT EXTRACTION

2002 ◽  
Vol 37 (2) ◽  
pp. 141-150 ◽  
Author(s):  
S. Tao ◽  
Y. H. Cui ◽  
J. Cao ◽  
F. L. Xu ◽  
R. Dawson ◽  
...  
Keyword(s):  
Solvent Extraction ◽  
Agricultural Soil ◽  
Accelerated Solvent Extraction

Determination of Felodipine in Tablets Using Accelerated Solvent Extraction

1998 ◽  
Vol 21 (4) ◽  
pp. 535-549 ◽  
Author(s):  
E. Björklund ◽  
M. Järemo ◽  
L. Mathiasson ◽  
L. Karlsson ◽  
J. T. Strode ◽  
...  
Keyword(s):  
Solvent Extraction ◽  
Accelerated Solvent Extraction

scholarly journals Development and validation of the method for the quantitative determination of methotrexate in a transport medium by HPLC-MS/MS

2021 ◽  
pp. 45-51
Author(s):  
P. Yu. Mylnikov ◽  
Yu. Tranova ◽  
A. V. Shchulkin ◽  
E. N. Yakusheva
Keyword(s):  
Quantitative Determination ◽  
Gradient Elution ◽  
Sample Volume ◽  
Transport Medium ◽  
Mass Selective Detector ◽  
Transporter Protein ◽  
Wide Range ◽  
Separation Temperature

Relevance. BCRP is an efflux transporter protein that plays an important role in the pharmacokinetics of a wide range of drugs. The BCRP activity in vitro experiments is assessed by the transport of transporter protein substrates (methotrexate, etc.) across the bilipid membrane of cells overexpressingBCRP, for example, Caco-2 cells. The aim is to develop and validate a method for the quantitative determination of the BCRP substrate, methotrexate, in the transport medium of Caco-2 cells by HPLC-MS/MS. Methods. The work was performed on an Ultimate 3000 HPLC chromatograph (ThermoFisher, USA) with a TSQ Fortis tandem mass-selective detector (ThermoFisher, USA). The conditions of chromatographic analysis were as follows: column UCT Selectra C18 4.6 mm * 100 mm 5um, 100A, Selectra C18 Guard Cartridges SLC-18GDC46-5UM, separation temperature 35 °С, flow rate 0.3 ml/min, injected sample volume - 2 μl, analysis time - 10 min. Used a gradient elution: the ratio of the solution of 0.1 % formic acid and acetonitrile was at 0 min 75 and 25 %; 0.4 min 60 and 40 %; 6 minutes 20 and 80 %; 8 minutes 75 and 25 %. Under these conditions, the retention time of methotrexate is 3.11 minutes. Detection conditions: methotrexate - positive ionization mode, 455.15 m / z → 308.125 m / z, collision energy 22.99 V, source fragmentation 5, CID gas pressure 2 mTorr. The extraction of methotrexate from the transport medium (Hanks solution with 25 mM Hepes and 1% dimethyl sulfoxide) after incubation with Caco-2 cells for 3 h was carried out with a mixture of methanol + water in a ratio of 1: 1. Results. The developed method was validated according to the following parameters: selectivity, linearity, accuracy, precision, limit of quantitative determination, sample transfer, sample stability. The confirmed analytical range of the method was 60 -10,000 nmol / L in the transport medium. Conclusions: a method for the quantitative determination of methotrexate in the transport medium of Caco-2 cells by HPLC-MS / MS was developed and validated.

scholarly journals Determination of Organochlorine Pesticides and Chlorobenzenes in Strawberries by Using Accelerated Solvent Extraction Combined with Sorptive Enrichment and Gas Chromatography/Mass Spectrometry

2001 ◽  
Vol 84 (4) ◽  
pp. 1194-1201 ◽  
Author(s):  
Luise Wennrich ◽  
Peter Popp ◽  
Gábor Köller ◽  
Jürgen Breuste
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solvent Extraction ◽  
Organochlorine Pesticides ◽  
Accelerated Solvent Extraction ◽  
Stir Bar Sorptive Extraction ◽  
Mass Spectrometry Analysis ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

Abstract An analytical scheme for the determination of several organochlorine pesticides like hexachlorocyclohexanes (HCHs) and DDX compounds (p,p′-DDE, p,p′-DDD, and p,p′-DDT) as well as chlorobenzenes in strawberries has been developed. The procedure is based on aqueous accelerated solvent extraction (ASE) followed by solidphase microextraction (SPME) or stir bar sorptive extraction (SBSE) and subsequent thermodesorption–gas chromatography/mass spectrometry analysis. A 65 μm polydimethylsiloxane/divinylbenzene fiber was chosen for the SPME experiments. Significant SPME and ASE parameters were optimized using spiked water and strawberry samples. For the ASE of the organochlorine compounds, a water–acetone mixture (90 + 10, v/v) as the extraction solvent, an extraction temperature of 120°C, and 2 cycles of 10 min extraction proved optimal. The developed method was evaluated with respect to precision and limits of detection (LOD). The relative standard deviations of replicate ASE–SPME determinations (n = 5) were in the range of 4–24%. LOD values between 1 and 10 μ g/kg were achieved with the exception of DDT and DDE (40 μg/kg). Using SBSE, the LOD of these compounds could be improved (2 and 5 μg/kg). The main advantages of this method are the avoidance of cleanup and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in strawberry samples collected from different allotment gardens in a potentially polluted area, the Bitterfeld-Wolfen region (Germany).

A Method for the Routine Determination of Corn Sirup in Prepared Meat Products

1964 ◽  
Vol 47 (5) ◽  
pp. 903-909
Author(s):  
Lester Hankin ◽  
Alphonse F Wickroski
Keyword(s):  
Statistical Analysis ◽  
Quantitative Determination ◽  
Correction Factor ◽  
Meat Products ◽  
Processed Meat ◽  
Average Amount ◽  
Wide Range ◽  
The Difference

Abstract A method has been devised for the determination of corn sirup added to processed meat products. The method is based on the quantitative determination of dextrin added to corn sirup. The dextrins are enzymatically hydrolyzed by α-amylase and β-amylase, and maltose is calculated as the difference in CuO2 found by copper reduction between a treated and an untreated aliquot. A correction factor was devised to determine the average amount of dextrin in corn sirup by testing a number of commercial sirups for their dextrin content and subjecting the data to statistical analysis. With this equation the method is applicable to a wide range of sirups. The method also permits the estimation of dextrose added to meats in excess of that included as one of the components of corn sirup.

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