Use of Solid-Phase Extraction Disks for Analysis of Moderately Polar and Nonpolar Pesticides in High-Moisture Foods

Casanova, John A

doi:10.1093/jaoac/79.4.936

Cited by 31 publications

(3 citation statements)

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“…The primary goal of the clean-up step was to use various sorbents to eliminate those co-extractives from the extract as much as feasible. Weak ion exchange is one of the sorbents that is most frequently utilised (PSA or –NH 2 ), Florisil, GCB and/or C 18 SPE sorbent [ 24 , 25 , 26 , 27 ]. The recoveries achieved using combination no.…”

Section: Resultsmentioning

confidence: 99%

Development of a Modified QuEChERS Method Coupled with LC-MS/MS for Determination of Spinetoram Residue in Soybean (Glycine max) and Cotton (Gossypium hirsutum)

Goon

Kundu

Ganguly

2022

JoX

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An analytical method for the quantitative determination of the insecticide spinetoram in cotton and soybean was established and validated using liquid chromatography tandem mass spectrometry (LC-MS/MS). Spinetoram is the mixture of two spinosyns, 3′-O-ethyl-5,6-dihydro spinosyn J and 3′-O-ethyl spinosyn L. The method involves extraction with ethyl acetate followed by dispersive solid phase extraction (dSPE) clean-up with primary secondary amine (PSA), C18 and graphitised carbon black (GCB). The final quantitation of spinetoram was done by using LC-MS/MS with positive electrospray ionization. The method was reproducible (Horwitz ratio (HorRat) < 0.5 at 25 ng g−1) and validated by the analysis of samples spiked at 25, 50 and 100 ng g−1 in soybean, cotton and soil. The recoveries of spinosyns were found to be more than 85% when spiked at different levels. The identities of spinosyns were confirmed by using the ion ratio. A field dissipation study was conducted in soybean and cotton to find out the environmental fate of spinetoram, and samples were analysed following the proposed analytical method. Both isomers were found to be dissipated quickly. The pre-harvest interval of spinetoram was calculated in different substrates.

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Section: Resultsmentioning

confidence: 99%

Development of a Modified QuEChERS Method Coupled with LC-MS/MS for Determination of Spinetoram Residue in Soybean (Glycine max) and Cotton (Gossypium hirsutum)

Goon

Kundu

Ganguly

2022

JoX

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“…SPE has been used extensively as a cleanup procedure for biological sample analysis (Casanova 1996). The separation mechanisms of SPE are the same as those for high-performance liquid chromatography.…”

Section: Resultsmentioning

confidence: 99%

“…This approach has distinctive advantages compared with the Soxhlet method, in that it employs size-exclusion chromatography to separate fat. SPE is also gaining popularity in pesticide analysis as it is finding greater application for replacing traditional liquid-liquid extraction (Casanova 1996). Two SPE columns that have been most often used are C18 and silica gel columns.…”

Section: Introductionmentioning

confidence: 99%

Linking Solid Phase Extraction and Enzyme‐Linked Immunosorbent Assay to Measure Chlorpyrifos in Fish Tissue

Wan¹,

Santerre²,

Deardorff³

2001

Journal of Food Science

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A method for measuring chlorpyrifos in fish tissue coupling solid phase extraction (SPE) and enzymelinked immunosorbent assay (ELISA) is described. Fish tissue was added to a silica gel column and extracted with hexane. The eluant was passed through an SPE column (C-18) and analyzed using ELISA. The method, which was comparable to an FDA GC/ECD method, gave recoveries from 83.4% to 87.5% for fortified fish samples, a lower limit of detection of 0.01 ppm, a linear range from 0.01 to 0.5 ppm, and correlation coefficients from 0.86 to 0.96. Nineteen contaminated fish samples analyzed using both ELISA and GC/ECD methods gave comparable chlorpyrifos concentrations with a correlation coefficient of 0.78.

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Matrix solid-phase dispersion extraction of organophosphorus and synthetic pyrethroid pesticides in cashew nut and passion fruit

Dórea

Lanças

1999

J. Micro. Sep.

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A multiresidue extraction method based on matrix solid‐phase dispersion (MSPD) and capillary gas chromatography–electron capture detection for quantification of five widely used organophosphorus insecticides (diazinon, malathion, parathion, methidathion, and pyrazophos) and one synthetic pyrethroid (permethrin) in Brazilian fruits is described. Cashew nut and passion fruit are plants native to South America. Capillary gas chromatography with mass selective detection was also utilized to confirm the pesticides through mass spectra. Different parameters were optimized, such as the solid phase and dispersant used, amounts, type of eluant and volume, and sample amount. The best results were obtained using a silica gel cartridge column and Florisil as dispersant. The eluant was ethyl acetate. Analysis of fortified fruit (n=3) shows an average recovery of 101.4% for cashew nut and 97.8% for passion fruit at 0.3–1.0‐mg/kg levels. Detection limits ranged from 0.2 to 0.4 pg for the compounds studied using 1‐g samples. The linearity, repeatability, and recoveries of the method are presented. This MSPD method was compared with solid‐phase extraction (SPE) for cleanup, using an alumina–silica gel (1 : 1) cartridge column and ethyl acetate as eluant. Analysis of fortified fruit (n=3) shows an average recovery of 104.9% for cashew nut and 106.8% for passion fruit at 0.1–0.6‐mg/kg levels. Detection limits ranged from 0.2 to 0.6 pg for the compounds studied using 25‐g samples. The combined use of C18 and silica (or Florisil) makes this extraction system unsuitable for these fruits matrixes. The cleanest extracts are obtained using two polar (Florisil and silica) solid phases. In conclusion, the proposed MSPD method described here can be applied to extract five organophosphorus pesticides and permethrin in 1 g of fruit. It is advantageous because it uses ethyl acetate as the only solvent, is faster and uses less solvent than SPE methods, and requires only small sample sizes. ©1999 John Wiley & Sons, Inc. J Micro Sep 11: 367–375, 1999

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Use of Solid-Phase Extraction Disks for Analysis of Moderately Polar and Nonpolar Pesticides in High-Moisture Foods

Cited by 31 publications

References 0 publications

Development of a Modified QuEChERS Method Coupled with LC-MS/MS for Determination of Spinetoram Residue in Soybean (Glycine max) and Cotton (Gossypium hirsutum)

Development of a Modified QuEChERS Method Coupled with LC-MS/MS for Determination of Spinetoram Residue in Soybean (Glycine max) and Cotton (Gossypium hirsutum)

Linking Solid Phase Extraction and Enzyme‐Linked Immunosorbent Assay to Measure Chlorpyrifos in Fish Tissue

Matrix solid-phase dispersion extraction of organophosphorus and synthetic pyrethroid pesticides in cashew nut and passion fruit

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