Determination of Twenty Organophosphorus Pesticides in Wheat Samples from Different Regions of Iran
Iranian Journal of Toxicology
Volume 11, No 5, September-October2017
Original Article
Determination of Twenty Organophosphorus Pesticides in Wheat Samples
from Different Regions of Iran
Attaollah Shakoori *1, Peyman Mahasti 2, Vahideh Moradi 2
Received: 10.01.2017
Accepted: 15.02.2017
ABSTRACT
Background: Organophosphorus pesticides are widely used in agriculture, homes, gardens, and
veterinary practices. Extensive application of pesticides in agriculture often results in residues of
these compounds being absorbed into the foods, including wheat. The aim of this study was to
evaluate the residue levels of 20 organophosphorus pesticides in wheat samples collected from
different regions of Iran.
Methods: This research reports a rapid, specific and sensitive multiresidue method based on the
Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas
chromatography with mass spectrometric detection in the selected ion monitoring mode (GC–
SIM–MS) to evaluate 20 organophosphorus pesticides in wheat samples.
Results: In the concentration range of 20-200 ng/g, the calibration curves for each analyte was
linear with a determination coefficient (R2) of 0.993 to 0.999. The limits of detection (LODs) and
quantitation (LOQs) were between 2.5-6.7 and 7.5-20 ng/g, respectively. The mean recoveries
obtained for three fortification levels (25, 50 and 100 ng/g, five replicates each) were 80-114% with
a satisfactory precision (RSD<20%). 31.1% samples contained residues of one or more target
compounds. Chlorpyrifos was the most common residue (17.8%), followed by pirimiphos-methyl
(6.7%), diazinon (4.4%), chlorpyrifos-methyl (1.1%) and malathion (1.1%).
Conclusion: Among the detected pesticides, only diazinon and malathion are permitted
pesticides for wheat production in Iran. However, their concentrations were below the maximum
residue levels (MRLs) established by the Iranian National Standard Organization (INSO).
Keywords: GC-MS, Organophosphates, Pesticides, Wheat.
IJT 2017 (5): 37-44
INTRODUCTION
Pesticides are natural or synthetic chemicals
used in agriculture to protect crops against
destructive pests. They are also used in public
health for the eradication of disease vectors and
other pests. Annually, at least 4 million tons of
pesticides are used for control of pests in the
world. Only 1% of applied pesticides reach the
target pests. Therefore, 99% of pesticides are left
in the environment; finally affect living organisms
[1]. Due to their widespread use, pesticides have
now become a major group of environmental
contaminants. They pollute the environment and
remain in food chains, thereby posing health
hazards to humans [2, 3]. Chemically, pesticides
belong to different classes and organophosphorus
pesticides constitute one of the major families,
highly potent compounds used mainly as
insecticides. Former restrictions on some
persistent pesticides had led to the use of nonpersistent alternatives such as organophosphorus
compounds, carbamates and pyrethroids, which
are very effective in pest control, in both
agricultural and residential settings [4]. Today,
organophosphates are the most widely used
pesticides across the world comprising 70% of the
compounds in use [5]. In 2007, nearly 35% of
applied insecticides in the US comprised
organophosphorus, worth about 33 million pounds
each year [6].
Intensive and extensive use of these
compounds is now posing a significant risk to
public health because of their potential adverse
effects. Exposure to organophosphates affects not
only those who use them occupationally, but the
1. PhD and Pharm D, Food Safety Research Center, Shahid Beheshti University of Medical Sciences, Tehran, Iran.
2. Department of Food Science and Technology, Science and Research Branch, Islamic Azad University, Tehran, Iran.
* Corresponding author: Email:
Iranian Journal of Toxicology
Attaollah Shakoori et al
general population exposed to low concentrations
of these compounds via foodstuffs and the
environment throughout their lifetime [7].
Organophosphate poisoning continues to be a
major cause of morbidity and mortality in third
world countries.
Chemically, organophosphates are esters of
phosphoric or thiophosphoric acids. They can
phosphorylate
the
active
site
of
acetylcholinesterase (AChE), which hydrolyses
acetylcholine (ACh) in cholinergic synapses and
in neuromuscular junctions. This excessive
accumulation of acetylcholine in synapses leads to
activation of cholinergic receptors [8]. Acute
effects of organophosphorus pesticides are well
documented. They can cause dizziness, headaches,
gastrointestinal distresses, bronchospasm, miosis,
urination, sweating, lacrimation, bradycardia,
fasciculations, muscle weakness, hypertension,
liver and kidney damage, coma and ultimately
death [9, 10]. However, some investigations have
revealed a number of organophosphorus
secondary targets not associated with the
cholinergic
system
and
may lead
to
immunotoxicity [11], endocrine disruption,
genotoxicity, and potential carcinogenic effects
such as non-Hodgkin’s lymphoma [12] and some
types of leukaemia [13]. Children may be more
vulnerable than adults may to the effects of
pesticides because of proportionally higher food
and water intake relative to body weight, along
with immaturity in the neurological development
and detoxification pathways [14].
Unlike acute poisoning, chronic exposure of
humans to small amounts of organophosphates
through the air and consumption of contaminated
food and water can affect a large proportion of the
population. Therefore, a pesticide residue in
foodstuffs continues to be the target of many
studies due to the mentioned adverse effects.
Several techniques are available for the
determination of these residues, but traditional
pesticide analysis procedures are complicated,
time-consuming and labor-intensive. In spite of
the variety and complications of the matrices and
low levels of pesticides in different food samples,
analysis and sample preparation techniques in the
area of pesticide residues have remarkably
progressed [15].
In 2003, a fast and easy
multiresidue technique was developed named
QuEChERS (Quick, Easy, Cheap, Effective,
Rugged, and Safe) method [16]. It is based on
initial single-phase extraction with acetonitrile,
followed by liquid–liquid partitioning by addition
of anhydrous magnesium sulfate (MgSO4) and
sodium chloride. Removal of the water content
and cleanup are achieved by MgSO4 and a primary
secondary amine (PSA) sorbent. This method is
very flexible and serves as a template for
determination of pesticide residues. Today,
combination of QuEChERS method and mass
spectrometry technique including LC-MS and
GC-MS, have been successfully applied to
determine the multiresidue levels of pesticides in
various food samples [17,18].
Wheat is one of the most common staple
foods in the world and especially in Iran. Most
pesticide residues in wheat are due to direct
application of pesticide duri (...truncated)