Multi-residue matrix solid-phase dispersion method for the determination of six synthetic pyrethroids in vegetables followed by gas chromatography with electron capture detection

1995 ◽  
Vol 695 (1) ◽  
pp. 75-82 ◽  
Author(s):  
Y.-C. Ling ◽  
I.-P. Huang
2001 ◽  
Vol 84 (4) ◽  
pp. 1165-1171 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo

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.


2001 ◽  
Vol 84 (5) ◽  
pp. 1561-1568 ◽  
Author(s):  
Cristina Yagüe ◽  
Susana Bayarri ◽  
Regina Lázaro ◽  
Pilar Conchello ◽  
Agustín Ariño ◽  
...  

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.


2006 ◽  
Vol 89 (5) ◽  
pp. 1425-1431 ◽  
Author(s):  
Christine J Akre ◽  
James D MacNeil

Abstract Synthetic pyrethroids are among the most widely used classes of insecticides, and their uses are varied, including plant protection, animal dips, and as a treatment for human clothing and bedding in very hot climates. Veterinary applications include ear tags, pour-on formulations, sprays, and dips. Persistent residues have been reported in livestock, and routine monitoring programs in other countries have found detectable residues of various pyrethroids in fat. A method has been developed using solid-phase extraction that reduces the quantities of solvents used, the time required, and the amount of glassware used compared to an earlier method on which it was based. The scope of analytes tested included the 5 compounds cited in the earlier method (flucythrinate, permethrin, cypermethrin, fenvalerate, and deltamethrin) and, in addition, cyfluthrin, λ-cyhalothrin, and fluvalinate. Sample extracts were analyzed by gas chromatography with electron capture detection using selected chromatographic peaks characteristic of each compound. Limits of quantification for the compounds were from 25-50 μg/kg, with a linear response for all compounds to 200 μg/kg. Recoveries ranged from 80 to 123%.


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