Single step clean-up and GC-MS quantification of organochlorine pesticide residues in spice powder

Abstract

SummaryLevels of fourteen organochlorine pesticides have been determined in ready-to-use spice powders. The pesticides were extracted with n-hexane-clichloromethane (4:1) and the extracts were cleaned in a single step on a cartridge packed with silica-and Florisil. The pesticides were quantified by GC-MS in SIM (selected ion monitoring) mode. Recoveries measured for pesticide-free spices ranged from 60% for dieldrin and enclrin to 97% for other pesticides. The relative standard deviation (RSD) of the method for all the pesticides was less than 15%. The method was applied to different spices (pepper, mace, and nutmeg). Methoxychlor, hnclane, and DDTancl its metabolites were found in all the samples; dieldrin and enclrin were not detected in any.spice ingredients [4]. Another approach must, therefore, be considered for the clean-up of spices.Solid-phase extraction on different adsorbents has been used successfully. Several papers have described the determination of organochlorine pesticides in medicinal plants [3], black tea [7], fresh fruit and vegetables [8], and in raw crops and animal feeds [9] by use of solvent extraction and solid-phase extraction [10,11]. Use of supercritical-fluid extraction (SFE) was recently reported for the extraction of organochlorine pesticides from chamomile [12].To the best of our knowledge, no comprehensive data are available on the monitoring of organochlorine pesticides in ready-to-use spice powder. The aim of this study was to develop a simple, rapid and accurate method for the determination of organochlorine residues in ready-to-use spices.

Multiresidue analysis of organochlorine and pyrethroid pesticides in ground beef meat by gas chromatography-mass spectrometry

“…The analytical methods developed for the determination of OCPs and PYRs involve traditional extraction techniques such as extraction by Soxhlet [2,3] and sonication [4,5] as well as modern extraction techniques such as supercritical fluid extraction (SFE), [6−9] microwave-assisted extraction (MAE), [10] accelerated solvent extraction (ASE) [2,11] Analysis of pesticides in ground beef meat 351 and extraction by Polytron. [2,12] SFE, MAE and ASE techniques work automatically and require low quantities of solvent, with a consequent reduction of solvent waste.…”

GC–MS determination of organochlorine pesticides in medicinal plants harvested in Brazil

“…The sample preparation (extraction and clean-up) was based on the procedure recommended by Manirakiza et al 9 for the determination of organochlorine pesticides in condiments by GC-ECD using, for clean-up, solid phase extraction with a mixed florisil/silica stationary phase and 10 mL n-hexane-dichloromethane (4:1 v/v) as elution solvent. Fortified samples of the three medicinal plants with the nine OCP under study were employed.…”

“…In general, the analytical method involves the following stages: sampling, sample preparation, extraction, detection and data analysis, where the sample preparation could be considered a critical step. The official multiresidue pesticide methods recommend extraction of the pesticides with organic solvents, 8 clean-up by column chromatography 4,9,10 or gel permeation chromatography 8,11 and quantification by capillary GC-MS. [12][13][14] Since the recommended extraction procedure requires large quantities of toxic solvents, other extraction procedures have been reported, including, solid-phase extraction, 9,10,15,16 supercritical fluid extraction 17 and microwave assisted extraction coupled to solid phase microextraction. 18 With relation to current Brazilian legislation, which regulates the registration of phytopharmaceuticals, the determination of pesticides has not been included in the purity assay of herbal plants.…”

Remediation of Dicofol Type Ddts-Contaminated Sediments by Ferrous Activated Sodium Persulfate Oxidation

“…Afterwards, column temperature was switched to a rate of 5 °C min -1 to 160 °C min -1 for 6 min, and then, to a rate of 10 °C min -1 to 190 °C for 3 min. Finally, the temperature was switched to a rate of 20 °C min -1 to 300 °C and maintained isothermally for 2 min (Manirakiza et al, 2000). The injection volume was 1.0 μL in a splitless mode.…”