Single step clean-up and GC-MS quantification of organochlorine pesticide residues in spice powder.
TL;DR: In this paper, the levels of fourteen organochlorine pesticides have been determined in ready-to-use spice powders using GC-MS in SIM (selected ion monitoring) mode.
Abstract: Levels of fourteen organochlorine pesticides have been determined in ready-to-use spice powders. The pesticides were extracted withn-hexane-dichloromethane (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 endrin 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, lindane, and DDT and its metabolites were found in all the samples; dieldrin and endrin were not detected in any.
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Journal Article•
TL;DR: Solid phase extraction (SPE) is an extraction method that uses a solid phase and a liquid phase to isolate one, or one type, of analyte from a solution as mentioned in this paper.
Abstract: Solid phase extraction (SPE) is an extraction method that uses a solid phase and a liquid phase to isolate one, or one type, of analyte from a solution. it is usually used to clean up a sample before using a chromatographic or other analytical method to quantify the amount of analyte(s) in the sample. The general procedure is to load a solution onto the SPE phase, wash away undesired components, and then wash off the desired analytes with another solvent into a collection tube. Solid-phase extractions use the same type of stationary phases as are used in liquid chromatography columns. The stationary phase is contained in a glass or plastic column above a frit or glass wool. The column might have a frit on top of the stationary phase and might also have a stopcock to control the flow of solvent through the column. Commercial SPE cartridges have 1-10 ml capacities and are discarded after use. it is usually used to clean up a sample before using a chromatographic or other analytical method to quantify the amount of analyte(s) in the sample. Solid phase extraction procedures are used not only to extract traces of organic compounds from environmental samples but also to remove the interfering components of the complex matrices in order to obtain a cleaner extract containing the analytes of interest. The SPE technique is widely applied for isolation of analytes from a liquid matrix and purified extracts. This paper is a review of the literature regarding general information about SPE technique, new trends in SPE technique and its application.
274 citations
TL;DR: The applicability of the method for the simultaneous determination of dyes, aflatoxins and pesticides in several types of spices was demonstrated, and the method successfully applied to a limited number of products from the local market.
Abstract: Based on several alerts from European countries over the last years concerning spices, we have been encouraged to establish an accurate method for the determination of dyes, aflatoxins and pesticides in various types of spices using reversed-phase (RP) liquid chromatography–tandem mass spectrometry interfaced with electrospray (LC–ESI–MS/MS). A simple sample treatment procedure entailing the use of an extraction step with acetonitrile without further cleanup has been developed. A C18 column with an aqueous ammonium formate/methanol mixture as the mobile phase was used, and gradient elution was performed. Mass spectral acquisition was done in positive ion mode by applying multiple reaction monitoring of at least two fragmentation transitions per compound to provide a high degree of selectivity. The method was in-house validated in terms of linearity, sensitivity, repeatability, recovery and selectivity on six kinds of spices. Satisfactory results in the majority of the cases were obtained for all analytes and matrices, with practical limits of quantitation acceptable for routine monitoring purposes. Extraction recoveries for most of the compounds ranged from 60% to 140% at spiking levels of 0.05 and 0.5 mg kg−1. The applicability of the method for the simultaneous determination of dyes, aflatoxins and pesticides in several types of spices was demonstrated, and the method successfully applied to a limited number of products from the local market.
120 citations
TL;DR: A method to determine 21 organochlorine pesticides in vegetation samples using microwave-assisted extraction (MAE) is described and compared with Soxhlet extraction, showing that both methods are suitable for the determination of chlorinated pesticides in Vegetation samples.
119 citations
TL;DR: In this article, a method was optimized and validated for the simultaneous determination of residues of organochlorine (OCP) and organophosphorus (OPPs) pesticides in meat samples from chicken, pork and lamb.
112 citations
TL;DR: A method to determine organochlorine pesticides in horticultural samples using pressurized liquid extraction (PLE) is described and compared with microwave assisted extraction (MAE), which showed low standard deviations for most of the studied pesticides.
76 citations
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TL;DR: The aging of HCH andDDT indicated a recent use of both pesticides during the potato storage period between cultivation seasons, however, such use is illegal because HCH mixture isomers (gammaxane) and DDT have been officially prohibited from agricultural use in Egypt since 1980.
Abstract: A market basket survey was conducted to monitor organochlorine and organophosphorus pesticide residues in potatoes, citrus fruits, and fish collected from local Egyptian markets. Maximum Residue Limits (MRLs) of the Codex Committee on Pesticide Residues for gamma-hexachlorocyclohexane (HCH) in potatoes were exceeded in 8 samples and for DDT in 2 samples. The aging of HCH and DDT indicated a recent use of both pesticides during the potato storage period between cultivation seasons. However, such use is illegal because HCH mixture isomers (gammaxane) and DDT have been officially prohibited from agricultural use in Egypt since 1980. The highest residue levels of fenitrothion (3.8 ppm) in potatoes may be due to its repeated use before and after harvest. No organochlorine pesticide residues were found in citrus fruits. None of the detected organophosphorus pesticides exceeded their MRLs. HCH and DDT residue limits were exceeded in 5 and 7 fish samples, respectively, collected from 12 markets throughout the country. The heptachlor MRL was violated in only one fish sample (3.9 ppm).
46 citations
TL;DR: In this paper, the application of various extraction solvents with an Ultra-Turrax system and ultrasonication with a probe and solid-phase extraction (SPE) with octadecyl (C 18 )-bonded silica and Florisil cartridges to linden samples for the gas chromatography-electron capture detection (GC-ECD) of α-hexachlorocyclohexane (α-HCH), β -HCH, γ-hCH, hexachlorobenzene (HCB), heptachlor and
43 citations
TL;DR: In this paper, a two-cartridge system composed of Extrelut-3 with a C18 cartridge connected downstream has been developed for the separation of organochlorine (OC) pesticide residues from oils and fats.
41 citations
TL;DR: In this article, a total of 44 pesticides were analysed by GC with electron capture detection, and the performance of cleanup with either C 18 or Floisil SPE were compared.
Abstract: Broccoli, carrot, celery, and orange, were fortified with a total of 44 pesticides. Pesticides were analysed by GC with electron capture detection. Performance of cleanup with either C 18 or Floisil SPE were compared
32 citations
TL;DR: Diatomaceous earth columns used with reversed and normal solid phase extraction (SPE) cartridges were evaluated for the quantitative determination of a number of organophosphorus (OP) and organochlorine (OC) pesticide residues in edible vegetable oils and butterfat.
Abstract: Diatomaceous earth columns used with reversed and normal solid phase extraction (SPE) cartridges were evaluated for the quantitative determination of a number of organophosphorus (OP) and organochlorine (OC) pesticide residues in edible vegetable oils and butterfat. An oil or fat sample (about 2 g) in hexane was passed through a diatomaceous earth (Extrelut QE) column and a C18 bonded silica (ODS) SPE cartridge, resulting in the separation of the pesticides from about 98% of the lipids. The eluate was split in half, with the first portion concentrated into acetone for the determination of OP pesticides by gas chromatography with flame photometric detection (GC-FPD). The other half was passed through an Alumina-N SPE cartridge for additional cleanup of lipid matrix to determine OC pesticides by GC with electron-capture detection (GC-ECD). Average recoveries from fortified samples were greater than 89% for the pesticides studied.
30 citations