scholarly journals Development and Validation of a HPLC-UV Method for Simultaneous Determination of Five Sulfonylurea Herbicide Residues in Groundnut Oil Followed by Matrix Solid-Phase Dispersion

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
T. Nageswara Rao ◽  
A. Ramesh ◽  
T. Parvathamma
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Solid Phase ◽  
Sulfonylurea Herbicide ◽  
Groundnut Oil ◽  
Herbicide Residues ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

A simple, sensitive, and inexpensive method was developed using matrix solid-phase dispersion (MSPD), together with high performance liquid chromatographic method for determination of sulfonylurea herbicide residues (nicosulfuron, pyrazosulfuron ethyl, metsulfuron methyl, chlorsulfuron and azimsulfuron) in groundnut oil. The evaluated parameters included the type and amount of sorbent (silica gel, C 18 and florisil) and the nature of eluent (ethyl acetate, dichloromethane, and acetonitrile). The best results were obtained using 1.0 g of groundnut oil sample, 1.0 g of C 18 as sorbent, and 20 mL of ethyl acetate-dichloromethane (1 : 1, (v/v)). The method was validated using groundnut oil samples spiked with sulfonylurea herbicides at different concentration levels (0.05 and 0.5 g/mL). Average recoveries (using each concentration six replicates) ranged 90–97%, with relative standard deviations less than 3%, the concentration of calibration solutions was in the range 0.01–2.0 g/mL and limits of detection (LOD) as well as limits of quantification (LOQ) were 0.01 g/mL and 0.05 g/mL, respectively.

scholarly journals Application of Matrix Solid-Phase Dispersion and High-Performance Liquid Chromatography for Determination of Sulfonamides in Honey

2008 ◽  
Vol 91 (1) ◽  
pp. 252-258 ◽  
Author(s):  
Qiong-Hui Zou ◽  
Jin Wang ◽  
Xiang-Feng Wang ◽  
Yuan Liu ◽  
Jie Han ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Solid Support ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Sulfonamide Residues

Abstract A novel method for simultaneous determination of 8 sulfonamide residues (sulfathiazole, sulfapyridine, sulfadiazine, sulfamerazine, sulfamonome-thoxine, sulfachloropyridazine, sulfamethoxazole, and sulfadimethoxine) in honey samples by high-performance liquid chromatography (HPLC) has been developed on the basis of precolumn derivatization with 9-fluorenylmethyl-chloroformate (FMOC-Cl). Sulfonamide residues in honey samples were extracted and purified by matrix solid-phase dispersion with C18 as the solid support. The residues were derivatized by FMOC-Cl, and the FMOC-sulfonamide derivatives were further purified by solid-phase extraction with silica gel as the solid support prior to HPLC analysis. The average recoveries for most sulfonamide compounds at different spiking levels (from 10 to 250 g/kg) were >70 with relative standard deviations <16, and their limits of detection were 4.0 g/kg. The established analytical method has high sensitivity and repeatability and can be applicable for determining the sulfonamide residues in various honey matrixes.

scholarly journals Determination of Insecticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Nitrogen–Phosphorus Detection and Mass Spectrometric Confirmation

2002 ◽  
Vol 85 (1) ◽  
pp. 128-133 ◽  
Author(s):  
Consuelo Sánchez-Brunete ◽  
Beatriz Albero ◽  
Ester Miguel ◽  
José Luis Tadeo
Keyword(s):  
Solid Phase ◽  
Single Step ◽  
Organophosphorus Insecticides ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
The Matrix ◽  
Low Volume ◽  
Nitrogen Phosphorus

Abstract A multiresidue method was developed for the determination of 12 organophosphorus insecticides (diazinon, parathion methyl, fenitrothion, pirimiphosmethyl, malathion, fenthion, chlorpyrifos, quinalphos, methidathion, ethion, azinphosmethyl, coumaphos), one carbamate (pirimicarb), and one amidine (amitraz) in unifloral and multifloral honeys. The analytical procedure was based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and subsequent extraction with a low volume of hexane–ethyl acetate (90 + 10, v/v), assisted by sonication. The insecticide residues were determined by capillary chromatography with nitrogen–phosphorus detection and confirmed by mass spectrometry. Average recoveries at the 0.05–0.5 μg/g levels were >80% for organophosphorus insecticides and about 60% for the other insecticides, pirimicarb and amitraz, with relative standard deviations <10%. The detection limit for the different insecticides ranged between 6 and 15 μg/kg. The main advantages of the proposed method are that extraction and cleanup are performed in a single step with a low volume of organic solvent. The method is simple, rapid, and less laborious than conventional methods. Several Spanish honeys were analyzed with the proposed method and no residues of the studied insecticides were found.

scholarly journals Rapid MSPD-LC–MS/MS Procedure for Determination of Pesticides in Potato Tubers

2020 ◽  
Vol 58 (9) ◽  
pp. 831-843
Author(s):  
Magdalena Danek ◽  
Marcin Sajdak ◽  
Joanna Płonka ◽  
Hanna Barchańska
Keyword(s):  
Analytical Procedure ◽  
Solid Phase ◽  
Potato Tubers ◽  
Limit Of Quantification ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Validation Parameters ◽  
Dispersion Technique

Abstract The program of potato protection recommended by the producers of agrochemicals requires application: thiamethoxam, lambda-cyhalothrin, deltamethrin, rimsulfuron and metalaxyl. Therefore, there is a risk that these pesticides are present in tubers, thus posing a toxicological risk to the consumer. In this respect, it is necessary to monitor the presence of these compounds in edible plants. Therefore, the aim of this paper was to develop a novel, simple and robust analytical procedure for simultaneous determination of above-mentioned pesticides in potato tubers. To develop an analytical procedure that fulfills SANTE demands, quick, easy, cheap, effective, rugged and safe method and matrix solid phase dispersion technique were investigated. The final determination was conducted by liquid chromatography with tandem mass spectrometry. The obtained experimental data were analyzed by analysis of variance. For the extraction of analytes, matrix solid phase dispersion with octadecyl sorbent and methanol as eluent was chosen, since it provides the validation parameters according to SANTE requirements (recovery: 77–111%, relative standard deviation: 1–10%, limit of quantification: 0.9–5.0 μg/kg). This innovative analytical procedure is a practical analytical tool, which was successfully proven by applying it for target pesticides determination in potato tuber samples of different varieties randomly chosen at local markets.

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