Optimization of matrix solid phase dispersion coupled with gas chromatography electron capture detection for determination of chlorinated pesticides in soil

Talanta ◽  
2012 ◽  
Vol 101 ◽  
pp. 504-509 ◽  
Author(s):  
Amir Salemi ◽  
Elham Shafiei ◽  
Maryam Vosough
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Chlorinated Pesticides ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion

scholarly journals Multiresidue Determination of Pesticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Electron-Capture Detection

2001 ◽  
Vol 84 (4) ◽  
pp. 1165-1171 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Solid Phase ◽  
Organophosphorus Compounds ◽  
Organophosphorus Pesticides ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

Abstract A multiresidue method was developed for the determination of 15 pesticides (organochlorines, organophosphorus compounds, pyrethroids, and other acaricides) in various commercial honeys (eucalyptus, lavender, orange, rosemary, and multifloral). The analytical procedure is based on the matrix solid-phase dispersion of honey in a mixture of Florisil and anhydrous sodium sulfate; the mixture is placed in small plastic columns and extracted with hexane–ethyl acetate (90 + 10, v/v). The pesticide residues are determined by capillary gas chromatography with electron-capture detection. Recoveries with the method at concentrations between 0.15 and 1.5 μg/g ranged from 80 to 113%, and relative standard deviations were <10% for all the pesticides studied. The pesticide detection limits were within the range 0.5–5 mg/kg for organochlorines, around 3 μg/kg for the chlorinated organophosphorus pesticides studied, near 15 μg/kg for fluvalinate, and about 3 μg/kg for the other pyrethroids.

scholarly journals Multiresidue Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Milk by Gas Chromatography with Electron-Capture Detection after Extraction by Matrix Solid-Phase Dispersion

2001 ◽  
Vol 84 (5) ◽  
pp. 1561-1568 ◽  
Author(s):  
Cristina Yagüe ◽  
Susana Bayarri ◽  
Regina Lázaro ◽  
Pilar Conchello ◽  
Agustín Ariño ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Organochlorine Pesticides ◽  
Electron Capture ◽  
Analytical Method ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Repeatability And Reproducibility

Abstract A multiresidue analytical method based on matrix solid-phase dispersion was developed to analyze liquid milk for 22 organochlorine pesticides (OCPs) and 6 polychlorinated biphenyls (PCBs). Initial extraction is performed by loading 3 mL milk onto a 2.0 g octadecyl (C18)-bonded silica cartridge with n-hexane as the eluant. Neutral alumina column chromatography with sodium sulfate as the drying agent is used for further cleanup. The eluate is concentrated to 0.5 mL, and target analytes are determined by capillary gas chromatography with electron-capture detection. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of milk samples fortified at 10 and 1 μg/L levels. Average recoveries were between 74 and 106% for all residues except β-HCH, β-endosulfan, and endosulfan sulfate. Both repeatability and reproducibility relative standard deviation values were < 22% for all residues. Detection limits ranged from 0.02 to 0.12 μg/L and quantitation limits were between 0.02 and 0.62 μg/L. The proposed analytical method may be used as a fast and simple procedure in routine determinations of OCPs and PCBs in milk.

Matrix Solid Phase Dispersion(MSPD) Extraction and Gas Chromatographic Screening of Nine Chlorinated Pesticides in Beef Fat

1991 ◽  
Vol 74 (3) ◽  
pp. 493-496 ◽  
Author(s):  
Austin R Long ◽  
Maher M Soliman ◽  
Steven A Barker
Keyword(s):  
Gas Chromatography ◽  
Solid Phase ◽  
Linear Regression Analysis ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Electron Capture Detection ◽  
Chlorinated Pesticides ◽  
Relative Percentage ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion

Abstract A multiresldue technique Is presented for the extraction and quantitative gas chromatographic screening of 9 insecticides (lindane, heptachlor, aldrin, heptachlor epoxide, p.p'-DDE, dleldrln, endrin, p,p'-TDE, and p.p'-DDT) as residues In beef fat. Beef fat was fortified by adding the 9 Insecticides, plus dlbutyl chlorendate as Internal standard, to 0.5 g portions of beef fat and blending with 2 g C18 (octadecylsllyl)-derivatlzed silica. The C18/fat matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisll. The insecticides were then eluted from the column with 8 mL acetonitrile, and a 2μL portion of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The acetonitrile eluate contained all of the pesticide analytes (31.25-500 ng/g) and was free of interfering co-extractants. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9969 (±0.0021) to 0.9999 (±0.0001). Average relative percentage recoveries (85 ± 3.4% to 102 ± 5.0%, n = 25 for each insecticide), inter-assay variability (6.0 ± 1.0% to 14.0 ± 6.7%, n = 25 for each insecticide), and intra-assay variability (2.5-5.1%, n = 5 for each insecticide) indicated that the methodology is acceptable for the extraction, determination, and screening of these residues in beef fat.

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