Abstract
Brazilian citrus essential oils (mandarin, orange, lemon, bergamot and tangerine) were analyzed for the determination of pesticides residues of organochlorine (aldrin, chlordane, dieldrin and dicofol) and organophosphorus (methyl chlorpyrifos, dimethoate, methidathion and methyl parathion) . A comparative study between gas chromatography-mass spectrometry in selective ion monitoring mode (GC-MS-SIM) and gas chromatography-electron capture detector (GC-ECD) was performed using solid phase extraction (SPE) with Florisil® cartridge for the pre-concentration of pesticides. The average recovery of pesticides was from 71 to 83% as determined by GC-MS-SIM analysis and 99 to 104% by GC-ECD. The limit of quantification was from 0.93 to 3.93 mg L-1 in GC-MS-SIM and 0.09 to 0.12 mg L-1 in GC-ECD. Fifteen samples of commercial Brazilian citrus essential oils were analyzed and six samples showed contamination with values above the maximum residue limit (MRL) allowed by the Codex Alimentarius.
Highlights
Citrus essential oils (EOs) are extracted by coldpressing the fruit pericarp and are important raw materials for cosmetic, pharmaceutical, food and cleaning product industries, among others.[1]
GC-MS-SIM and gas chromatography-electron capture detector (GC-ECD) chromatograms of the pesticide fortified solutions, in each type of EO, were obtained and the peak identifications were confirmed by injecting different concentrations of the pesticides
The pesticide chlordane can present 26 isomers, but only areas of two peaks increased by the fortification of the EO
Summary
Citrus essential oils (EOs) are extracted by coldpressing the fruit pericarp and are important raw materials for cosmetic, pharmaceutical, food and cleaning product industries, among others.[1]. Di Bella et al.[4,5,6,7,8] investigated Italian citrus EOs from 1996 to 2004, and found 60 mg L-1 of chloroparaffin residue in lemon oil, above the level allowed by the Codex Alimentarius (7.1 mg L-1).[5] This group observed a dicofol contamination of 1.96 mg L-1 in mandarin EO and 0.20 mg L-1 of the same organochlorine in bergamot EO.[7] In 2004, a second study noted the presence of pesticides, but at levels below MRL.[8] Dellacassa et al.[9] analyzed organochlorine and organophosphorus residues in lemon EO from Uruguay. Contamination of methyl chlorpyrifos, methyl parathion, fenitrothion and methidathion was found in the EOs produced before 1993, but a strong reduction in the residues was observed after that year.[9] These studies highlight the importance of the constant monitoring of pesticide residues in agricultural-based products, as well as the need for development of methodologies with higher sensitivity, precision and accuracy. Baker®, lot 7213-07, USA), containing 1 g of adsorbent, were used
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