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ISSN-1996-918X
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017) 37 – 45
http://doi.org/10.21743/pjaec/2017.06.03
Pesticides Residue in Milk and Milk Products: Mini Review
Shazia Akhtar*1and Karam Ahad2
1*Ecotoxicology Research Institute, NARC, Islamabad, Pakistan.
2Ecotoxicology Research Institute, NARC, Islamabad, Pakistan.
*Corresponding author E-mail: shazoo_786@yahoo.com
Received 10 September 2016, Revised 14 June 2017, Accepted 23 June 2017
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Abstract
Livestock is an important sub-sector of agriculture that plays a key role in economy of a country
by contributing to GDP (Gross Domestic Product) and in total export. Pakistan is the 5th largest
milk producer in the world with a total milk production of about 46.44 billion liters per anum.
Almost 68% milk is produced by buffalo and 27% by cow. Pesticides used in agriculture sector
may transfer to animal bodies through feed and fodder. A pesticide found in water is another
source of residues in milk through drinking water. External control of parasites on animal body,
insect control in cattle yard and sheds are direct sources of pesticides exposure for dairy animals.
Due to its nutritional and supplementary value, milk is being consumed by people of different age
groups therefore, issue of pesticide residues attain the immediate attention of researcher. Pesticide
residues levels in raw dairy milk are discussed here in few selected developing and developed
countries. It is concluded that human health is associated with exposure to organo phosphorus
(OPPs), organo chlorine pesticide (OCPs), pyrethroids and carbamate (CB) pesticides via milk or
milk products and this issue deserve more attention. Different classes of pesticides OPPs, OCPs,
pyrethroids and CBs etc. were reported in raw dairy milk in different countries and also in
Pakistan. The results of this review demonstrate the need to establish pesticide residue monitoring
programs for milk analysis for human consumption to improve food safety and decrease exposure
risks to consumers.
Keywords: Pesticides residues, Organochlorine pesticide, Organophosphorus pesticide, Milk,
Maximum residues levels.
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Introduction
Pakistan is an agricultural developing country. Its
economy is mainly based on agriculture and
livestock that play an important role. About 30 to
35 million population is involved in livestock.
Overall in rural areas every family has cattle, goats
and buffalo. From these animals people receive
their 30 to 40% income. Almost 68% milk is being
produced by buffalo, 27% from cow and 5% from
goat, sheep and camel. Buffalo is main animal
contributing to milk production. Pesticides entere
in the human body through food, which have
animal origin especially richin lipid content rich.
Livestock is an important sector in Pakistan [1].
Some studies report that animal origin food is
responsible for 90% pesticides entry in the human
body [2]. Milk has nutritional and supplementary
value as well as it is being consumed by peoples of
different age groups therefore, this issue attain the
immediate attention of researcher. Since, milk
contains a considerable amount of fat, therefore
presence of these lipophilic compounds in it is
beyond any suspicion. Presence of pesticides in
milk was reported by several authors in different
countries over the last few decades, and use of
most of these chemicals had been banned in many
countries [3].
Sources of pesticide residues in milk
In agriculture, crops like fruits, vegetables
and cereals are treated with different types of
synthetic chemicals, which are known as pesticides
Mini
Review Paper
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017)
38
[4]. Pesticides include insecticides, herbicides,
rodenticides and fungicides etc. These pesticides
are applied pre-harvest, post harvest and storage
stages. They have ability to transfer from lower
plants and animals to the higher plants and animals
among the food chain and can accumulate in the
higher organisms [5]. In addition to this,
sometimes pesticides are directly sprayed to the
animal accommodation to infest the pest [6].
Ultimately, both routes (plants and animals) lead to
the bioaccumulation of pesticides in the animal
products like milk, meat, fat and eggs. Pesticides
source in dietary rout is main way of chronic
exposure to these substances [7, 8].
Analytical methodologies for pesticide residues
There are different techniques used for
pesticide residues analysis in milk. Gas
chromatography (GC) as well as liquid
chromatography (LC) is being used as separation
technique coupled with some detectors. Ideal
detectors used for the detection and quantification
of pesticide residues would respond only to target
analyte, while other coextracted elements remain
transparent [9].
Gas chromatography has been used with
different detectors like electron capture detector
(ECD), micro- ECD (μ-ECD), GC-NPD (nitrogen
phosphorus detector) and Flame ionization detector
(FID). Mass spectrometric detector (MSD) is
termed as the universal detector on the basis of its
non-specific properties. MSD being versatile and
selective detector is preferred by analyst [10].
LC-MS and LC-MS/MS is an ideal,
extremely specific and highly sensitive technique
used for identification and quantification of
pesticide residues. It provides information about
analyte without derivatizing. It can compensate
sample purity and it enables simultaneous analysis
of the compounds with varying polarity [11].
Public health concerns
A wide range of milk and milk products
are consumed by the peoples of all ages. From
polluted grass, corn, silage and through pesticides
direct application on cattle, these chemicals
accumulate in the cattle milk. As humans beings
are on the top of tropic level or in the food chain,
they are bigger consumers of pesticides. Products
of animal origin: meat, fish, eggs and especially
dairy products are main source of OCPs and OPPs
intake in general public [12]. These pesticides
cause a wide range of toxic effects and pose very
severe health risks, specifically in infants, who
have less developed metabolic and enzymatic
systems [13]. Overall health effects on humans by
pesticides are not well defined but evidences are
increasing for genotoxicity, carcinogenity and
hormonal disturbance [14, 15].
Milk has been analyzed as an indicator of
the bio-concentration for the persistent organic
pollutant like pesticides [16]. A class of
pesticides, organo chlorine, which are lipophilic
and has little metabolism in the body of living
animals. Environmental exposure of organo
chlorines leads to their accumulation in fats tissues
and magnify in living tissues through the food
chain [17].
Status of pesticide residues in milk and milk
products
This review covers the level of pesticides
contamination in different countries especially in
developing countries. In this regard, Pandit [18]
monitored milk samples of different brands in
Maharashtra, India to check the pesticide residues
contamination. Analysis was done with GC
technique with µ ECD. Hexachlorocyclohexane
(HCH) and di-chlorodiphenyltri-chloroethane
(DDT) were detected in trace amount in milk
samples. Overall HCH level was lower than DDT.
This may be due to anti-malarial sanitary activities.
Results showed that butter have higher
concentration of DDT than milk and cheese.
However, Organo chlorine pesticides levels were
blow the FAO (Food and Agriculture
Organization)/ WHO (World Health Organization)
standards.
It was investigated in a study, cow and
buffalo milk samples were collected from 6
different markets of Menia El-Kamh province of
the Sharkia Governorate constitutes, one of the
largest agricultural area in the Egypt. Thirteen
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017) 39
different pesticides were analyzed by High
performance liquid chromatography (HPLC) and
DDT, Larvin, Anifose and methomyl were
detected in milk samples and their concentrations
as high as 67 μg/kg (larvin), 88 μg/kg (anilifos),
138 μg/kg (DDT), and 325 μg/kg (methomyl) were
found in cow or buffallo milk [19].
Another monitoring study was carried on
to check the HCH and DDT. As chemicals are
extensively being used in public health and
livestock programs in the central tropical region in
Mexico. Milk samples were collected from
Tlalixcoyan and analyzed HCH and DDT. Results
demonstrate the mean level of HCH was
significantly higher than residues in milk samples
from Medellin (0.049 mg/kg-1) and Paso San Juan
(0.022 mg/kg-1). The DDT mean level from
Medellin milk samples (0.089 mg/kg-1) was
significantly higher than the levels detected in the
other two areas. These results showed that infants
are at more risk of exposure to pesticides residues.
These findings indicate that those cattle exposed to
DDT and HCH accumulates these chemicals in
their milk and may pose health risk to the
consumer [20].
Pagliuca et al. [21] described that OPPs,
which are being used in agricultural system, they
can accumulate in food chain and ultimately pose
toxic effects on animals and human beings. In Italy
a research was carried out conducted to determine
the OPPs in dairy milk and to adopt the special
procedure for risk management in the whole milk
production chain. Milk samples were collected
from tanks trucks of four dairy plants in Italy,
which were representations of 920 tons of raw
milk. The separation of the 8 OPPs (acephate,
chlorpyriphos, chlorpyriphos-methyl, diazinon,
methamidophos, methidathion, phorate,
pirimiphos-methyl) was done through liquid
partition and then clean-up with solid phase
extraction. Gas chromatography with Nitrogen
phosphorus detector (NPD) was used for detection
analysis. Total 135 samples were analyzed and 37
showed positive results and 10 were contaminated
with OPPs (5-18mg/kg). Acephate and
chlorpyriphos was main contaminant. However,
OPPs level of contamination was lower than MRLs
given by European Commission (EC).
Weber [22] stated that OCPs are not
readily degradable and are lipophilic in nature.
That is why OCPs have tendency to bio-
accumulate in fatty foods like milk. After a long
exposure to OCPs adverse type of health effects
may develop. Although it is banned in some
countries even then its residues are being found
and OCPs accumulation in fatty foods is a major
concern.
A method was developed for trichlorfon
residue as dichlorovos analysis by GC-µECD.
Dichlorovos confirmation was done by mass
spectroscopy. In this protocol acetonitrile was used
for milk extraction then centrifugation followed by
freezing and partitioning in dichloromethane. Ethyl
acetate was used for dissolution of residues for
GC. Average recoveries were noticed from 92.4%
-103.6%. No any residue was detected in milk
samples collected from seven major cities of Korea
[23].
During the handling and processing, milk
and milk products could be contaminated. Buffalos
and cow milk was investigated for pesticides
residue in Egypt. OPPs (profenofos, malathio,
pirimiphos-methyle and dimethoate) were not
detected in any milk sample. However, OCPs
(lindane, aldrin, heptachlor, epoxide, HCB, eldrin,
chlordane and DDT) were present above the
recommended limit established by FAO/WHO
[13].
Milk and feedstuff of goats and sheep was
monitored in a research. Total 200 milk samples
were collected from 10 goat and 10 sheep farms.
Milk samples were analyzed for 99 multi residues
by GC-MS (GC- Mass Spectrometry) and LC-
MS/MS (LC-Liquid chromatography) systems.
Feedstuff samples were contaminated with
pesticides residues; however milk, samples were
contaminated but found under safe limits [24].
Another study was reported by
Karabasanavar & Singh [25] for public health and
plants defense against pest, pesticides are being
used. Entrance of these pesticides to the food chain
is very harmful. Application of chloropyrifos in
the agricultural and associated fields leads to the
pesticides accumulation in milk also. A study was
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017)
40
designed to determine the chloropyrifos
concentration in milk. For this purpose milk
samples were collected from Kumaon and Tarai of
Uttarakhand state. HPLC technique was used to
analyze the milk samples. Total 170 samples were
analyzed and out of which 4.7% milk samples
were detected with chloropyrifos residues which
were also above the MRLs (0.02 mg/kg-1).
It was investigated OCPs in dairy milk
produced by buffalos, cows and sheep. 21
different types of pesticides were present in milk
and beta-HCH was more dominant in all collected
samples. Some pesticides were above the MRLs
recommended by European Union [26].
In another study [27] 30 raw milk samples
were collected from 28 different dairy farms in
August 2007 from Spain. Extraction of raw milk
samples was done by following the protocol of
Pagliuca et al. [21] and analyzed through gas
chromatography. The main pesticide was fenthion,
detected in four samples of 12 (33.33%), followed
by dimethoate (25%), coumaphos (8.33%) and
malathion (8.33%). In Carbamate group, the
pesticides detected were carbofuran (25%),
aldicarb (16.67%) and carbaryl (8.33%). In some
samples, two or more active principals were
detected, what explains percentages over 100%.
The frequency of pesticides found in this study is
in agreement with Araujo et al. [28] that noted that
the most pesticides commonly used in Pernambuco
are from OP class, followed by CB and
pyrethroids. The frequency of samples positive to
OPPs and CB residues was lower than the one
found by Nero et al. [29] that verified 196
(93.8%) positive samples among 209 raw milk
samples in four Brazilian regions. Thin Layer
Chromatography, which would justify the
difference in the results, since this technique
presents lower specificity when compared with
GC.
Pasteurized and fresh milk samples were
tested for OCPs by using GC with ECD in
Kampala. Aldrin, Lindane, Dieldrin, DDT and
Endosulfan were detected in milk. Results showed
that most of the residues detected were above the
residue limits set by the FAO/WHO (2008).
Bioaccumulation of these residues is likely to pose
health risks to the consumers of milk in Uganda
[30].
Aslam et al. planned a research to analyze
the OC residues and their chemical composition in
milk of buffalo. Milk samples were collected from
Dehli.Monitoring of milk could be useful for
getting information about the type and quantity of
OC residues in environment and in our daily life
also. The results indicated that p,p’-DDT was
exceeded in 70% of milk sample, p,p’-DDE in
80% of the milk samples of in Delhi state.
Dichlorodiphenyldichloroethane (DDD) another
metabolite of p,p’-DDT was also present in 65% of
the milk samples. The results revealed that DDT
was the main contaminant in Dehli state.
Endosulfan was detected in 35% milk samples.
Mixture of toxic compounds present in buffalo
milk samples might possibly toxic for infant’s
health mainly nervous system, reproductive and
immune system [31].
Another study was carried out in Mexico
where 40 milk samples were analyzed. It was
noticed that mostly OCPs were below the MRLs
adopted by Mexican regulations. However, HCH
and Heptachlor was above the MRLs of Codex
Alimentarius. It was also assessed that in future
goat milk will be safer for human consumption
and it is good alternative to livestock milk.
Contineous monitoring for HCH is required
through management practices [32].
In an another study, it was reported that 16
OPPs residues were determined in Tizayuca,
Hidalgo, Mexico during 2008-2010. GC with ECD
was used for OCPs determination and residues
concentrations were found higher in wet season
than dry season. Overall pesticides residues were
below the MRLs proposed by Codex Alimentarius.
This reduction in residues reflects that Mexican
government has achieved the safety levels in
response to persistent organic pollutants (POPs)
agreement [33].
Ayoub and coworkers conducted a study in
Egypt. They analyzed 72 buffalo milk samples for
OCPs and the only detected pesticide was p,p-
DDE. Maximum concentration was found 4.714
ppb but overall samples were below the MRLs
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017) 41
recommended by Codex Alimentarius Commission
(2004) [34].
In Brazil CBs and OPPs were investigated
in feedstuff, water and dairy milk. GC with NPD
was used to analyze these compounds. Total 30
milk samples were analyzed out of which 17%
samples were contaminated with OPPS. CBs were
not present in milk however, they were present in
feedstuff and water samples. Same ingredient was
noticed in 3 dairy farms [35].
A study was carried out to find the OCPs
and OPPs residues in milk and fodder samples
around the Musi river belt in India. Milk and
fodder samples were collected from different six
location of Musi river belt in Hyderabad, India.
Collected samples were analyzed by GC with ECD
for OCPs and pulsated flame photometric detector
(FPD) was used for the detection of OPPs residues.
Analysis of fodder showed dicofol concentration
ranging from 0.071-0.077 (0.07). Dimetheoate
(OPPs) was found in milk samples ranging from
0.111-0.167 (0.13). Residues of other OPPs and
OCPs were below the MRLs specified by
European Union (EU) and Codex. Whereas fodder
dicofol and in milk dimethoate were above the
MRLs values established by EU and CODEX [36].
It was reported in a study that fresh milk of buffalo
collected from agro-industrial zone in upper Egypt
was analyzed for OCPs and OPPs by using GC.
Five different OCPs (alachlor, HCB dieldrin,
methxychlor and linadane) and three different
OPPs (malathion, parathion-methyl and
chlorpyrifos) were identified in fresh milk samples.
It was found that Malathion and Lindane exceeded
permissible limit set by EU established in 2008
[37].
In addition to this, chloropyrifos, HCB and
methoxychlor were exceeded in 33%, 88% and
66%, respectively. However, parathion-methyl,
alachlor and dieldrin were below the MRLs
established by EC. Overall it was concluded that
Egypt peoples are at the risk of pesticides exposure
based on this, it was recommended that pesticides
monitoring programs should be established in all
developing countries.
Non- judicious use of pesticides leads to
contamination of food commodities with pesticide
residues. Although, pesticides consumption in
India is 0.5 kg/ha. A survey was conducted to
analyze the levels of OCPs residues in cow milk
from different locations of Dhanbad city,
Jharkhand, India. Milk samples were collected
seasonally, and pesticide residues were assessed
using gas chromatography with an electron capture
detector. The results indicate that the milk samples
were contaminated with DDT and its metabolites
(DDE and DDD). Seasonal variations of these
pesticide residue levels were also observed
in all the milk samples. Samples collected
during winter season were found to contain
higher residue levels as compared to other seasons
[38].
Ismail and Elkassas, carried out a survey to
analyze the concentrations of OCPs, OPPs and
Pyrethroids pesticides in milk of buffalos. The
findings demonstrate that OCPs were present with
high levels and their concentration exceeds the
FAO/WHO and EU MRLs. OPPs detection
levels were higher than MRLs established by
FAO /WHO. Cypermethrin and pyrethroid
concentrations were exceeded the FAO/WHO and
EU limits. This survey suggests the proper
monitoring of milk is required to keep consumers
safe [39].
Muhammad and his co workers conducted
a study in Faisalabad, where cattle milk was
collected from different localities of Faisalabad,
Pakistan and solid phase micro-extraction was
done for pesticides residue analysis and residues
were determined by using HPLC. The results of
this study revealed that overall 40% samples
showed pesticides contamination. The mean levels
of cypermethrin, chloropyrifos, endosulphane and
syhalothrin were 0.085, 0.072, 0.26 and 0.38
µg/mL, respectively. Pesticides residues risk
analysis was calculated on the bases of provisional
acceptable daily intakes and analyzed pesticides
residues. The daily intake levels of pesticide
residues including cyhalothrin, chlorpyrifos and
cypermethrin in present study were 3, 11, 2.5 times
higher, respectively in cattle milk. These results
showed that pesticides residues present in the milk
might pose health problems in the people of this
vicinity [40].
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017)
42
Country Year No. of
Samples No. of
samples
contaminated
(%)
No. of samples
above the MRLs
(%)
Pesticides detected Analytical method Reference
India 2002 54 - 60 HCH and DDT GC with µECD 18
Mexico 2003 240 - 70 HCH and DDT GC with ECD 20
Italy 2006 135 - 56 Acephate, chlorpyriphos, chlorpyriphos-methyl, phorate,
pirimiphos-methyl,diazinon, methamidophos, methidathion, GC with NPD 21
India 2007 - 75 - 2,4 DDE , 4,4 DDE, Aldrin, Dieldrin, BHC, Endosulfan ,Methyl
Parathion, Malathion, Dimethoate GC with ECD 3
Egypt 2015 120 - 100 OPPs GC with µECD and
FID 13
Korea 2011 12 - - Trichlorfon residue as dichlorovos GC with µECD 23
Uganda 2011 101 90 80 Aldrin, dieldrin, endosulfan, lindane, DDT and its metabolites GC-MS 30
Uttarakhand
state. 2013 170 - 4.71 Chloropyrifose GC with µECD 25
Turkey 2011 - - 5 16 OCPs GC with µECD 26
Egypt 2012 72 50 0 p,p’-DDE GC equipped with
double Electron
Capture Detectors
34
Pakistan
(Faisalab-ad) 2012 - 50 25 Cypermethrin, chloropyrifos, endosulphane and syhalothrin HPLC 40
India (Delhi) 2013 20 - 80 p,p’-DDT, p,p’-DDE, DDD and Endosulfan GC with µECD 31
Pakistan
(Lahore) 2013 140 50 50 Insecticides and OPPs HPTLC, UV and
GC-MS 41
Pakistan 2014 80 - 40 Insecticides and OPPs GC-MS 42
Mexico 2013 40 - 50 OCPs GC-ECD 32
Mexico 2015 - - 0 16 OPPs GC-ECD 33
Pakistan
(Punjab) 2014 150 70 70 Aldrin,bifenthrin, cypermethrin,endosulfan, deltamethrin,
permethrin,Dichlorodiphenyldichloro ethylene and
Dichlorodiphenyltricthloro ethane.
HPLC 24
Brazil 2014 30 - 16.67 OPPs and CBs GC-NPD 35
Egypt 2015 200 - 44 5 OCPs and 3 OPPs GC 37
Egypt 2016 - - 100 OCP and OPP and pyrethoid GC 39
Table 1. Status of pesticides residues in milk in different countries
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017) 43
Shahzadi and her co researchers
identified and quantified the insecticide
imidacloprid, pyrethroid (bifenthrin, deltamethrin
and lambda cyhalothrin), and OPP (chlorpyrifos)
in buffalo, sheep, cow, goat and camel milk. Milk
samples were collected from different locations
of Lahore in Pakistan. High performance thin
layer chromatography (HPTLC), Ultraviolet–
visible (UV) and GC-MS were used to analyze
the residues contamination level. These pesticides
residues were extracted with petroleum ether,
ethanol and sodium oxalate. Results indicate 50
% of the milk samples were contaminated with
pesticides residues. Most significantly present
pesticides were Deltamethrin and maximum
contamination was found in sheep milk. Milk
consumption contaminated with pesticide might
pose health hazardous to humans in this locality
[41].
In dairy farms present in peri-urban
areas, cattle are being fed on agro-industrial by
products diet (cotton khal, sugarcane khal, wheat
bran etc.) this activity may transfer chemicals to
cattle milk. In a similar type of study [42]
pyrethroid and OPPs were assessed. These
pesticides when accumulated in the fat tissues
and milk, they may pose adverse health risks to
human’s health. In the present study 30 diet and
80 milk samples were collected from different
dairy farms. All the samples were processed
through QuECHERS kit and analyzed by using
GC coupled with mass spectroscopy. The results
revealed that cypermethrin and chloropyrifos
concentrations were above the MRLs in 40%
milk samples proposed by WHO. Profenofos was
exceeded in the 20% milk samples.
It was reported in a research in Pakistan
in which pesticides residue levels was monitored
in milk of cattle from cotton growing areas of
Punjab. Analyzed pesticides were aldrin,
bifenthrin, cypermethrin, endosulfan,
deltamethrin, permethrin, DDD and DDT. HPLC
technique was used and findings showed that
70% milk samples showed exceeded level of
pesticides residues. Maximum contamination was
shown by Aldrin (0.68 µg/mL). Overall results
indicated that 23%, 21%, 18% and 7% of the
milk samples were contaminated with
cypermethrin, bifenthrin, permethrin and
detlamethrin, respectively [43].
Prevention and control of pesticide residues
Maximum residues levels (MRLs) have
been set by the European Union and Codex
Alimentareous to ensure that pesticides are
present below the unacceptable risk limit. These
MRLs are the upper legal limits of pesticides
concentrations in feed and food. MRLs are
established for a wide variety of plants and
animal’s origin based food commodities. MRLs
are not simply set as threshold levels of
toxicologically, but they are derived after a broad
assessment of the active substance properties and
their residue behavior on treated crops [44].
There was a need to investigate the pesticides
residues in milk in order to provide a baseline to
health department or governing bodies to make
safety regulations. In addition to this, pesticides
residues monitoring program is very essential for
the safety of consumer health and to achieve the
food safety in country.
Conclusion and recommendations
On the basis of above review worldwide
including Pakistan, it is concluded that human
health is associated with exposure to OCPs, OPPs
and pyrethroids pesticides via milk or milk
products and this issue deserve more attention.
Several OPPs and OCPs pesticide residues were
detected in raw animal milk samples collected
from different sources in Pakistan.
The results of this review demonstrate
the need to establish pesticide residue monitoring
programs for milk analysis for human
consumption to improve food safety and decrease
exposure risks for consumers. In addition to this,
these finding suggest creating awareness in
owner of dairy farms and general public
regarding the avoidance of pesticide residues in
milk.
References
1. H. Rana, M. F. Khan, M. F. Akbar, Z.
Ahmed, K. Mahmood, S. Eijaz and W.
Khan, Int. J. Biol. Res, 2, (2014) 45.
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017)
44
2. F. Tecles, A. Tvarijonaviciute and J. J.
Cerón, Pak. Vet. J., 33 (2013) 458.
3. S. K. Nag, S. K. Mahanta, M. K. Raikwar
and B. K. Bhadoria, Small Ruminant
Res., 67 (2007) 235.
https://doi.org/10.1016/j.smallrumres.2005.
10.008
4. A. N. Díaz and M. R. Peinado, Sens.
Actuators B., 39 (1997) 426.
https://doi.org/10.1016/S0925-
4005(97)00025-7
5. K. C. Jones and P. De Voogt, Environ.
Pollut., 100 (1999) 209.
https://doi.org/10.1016/S0269-
7491(99)00098-6
6. P. Stefanelli, A. Santilio, L. Cataldi and R.
Dommarco, J. Environ. Sci. Health B, 44
(2009) 350.
https://doi.org/10.1080/0360123090280100
0
7. S. Tao, W. X. Liu, X. Q. Li, D. X. Zhou, X.
Li, Y. F. Yang R. M. Coveney, Environ.
Pollut., 157 (2009) 497.
https://doi.org/10.1016/j.envpol.2008.09.00
5
8. S. Muralidharan, V. Dhananjayan and P.
Jayanthi, Environ. Res., 109 (2009) 15.
https://doi.org/10.1016/j.envres.2008.08.00
6
9. M. LeDoux, J. Chromatogr. A, 1218 (2011)
1021.
https://doi.org/10.1016/j.chroma.2010.12.0
97
10. L. Alder, K. Greulich, G. Kempe and B.
Vieth, Mass Spectrom. Rev., 25 (2006) 838.
https://doi.org/10.1002/mas.20091
11. S. J. Lehotay, K. Maštovská and S. J.
Yun, J. AOAC Int., 88 (2005) 630.
12. J. Falandysz, B. Wyrzykowska, J.
Warzocha, I. Barska, A. Garbacik-
Wesołowska and P. Szefer, Food Chem., 87
(2004) 17.
https://doi.org/10.1016/j.foodchem.2003.10
.011
13. E. M. Shaker and E. E. Elsharkawy,
Environ. Toxicol. Pharmacol., 39 (2015)
433.
https://doi.org/10.1016/j.etap.2014.12.005
14. I. Baranowska, H. Barchańska and E.
Pacak, Environ. Pollut., 143 (2006) 206.
https://doi.org/10.1016/j.envpol.2005.11.03
9
15. M. Fontcuberta, J. F. Arqués, J. R. Villalbi,
M. Martínez, F. Centrich, E. Serrahima and
C. Casas, Sci. Total Environ., 389 (2008)
52.
https://doi.org/10.1016/j.scitotenv.2007.08.
043
16. E. Kampire, B. T. Kiremire, S. A. Nyanzi,
and M. Kishimba, Chemosphere, 84 (2011)
923.
https://doi.org/10.1016/j.chemosphere.2011
.06.011
17. K. Borgå, G. W. Gabrielsen, J. U. Skaare,
Environ. Pollut., 113 (2001) 187.
https://doi.org/10.1016/S0269-
7491(00)00171-8
18. G. G. Pandit, S. Sharma, P. K. Srivastava,
and S. K. Sahu, Food Addit. Contam. 19
(2002) 153.
https://doi.org/10.1080/0265203011008115
5
19. H. Dahshan, A. M. Megahed,A. M M.
Abd-Elall, M. A. G. Abd-El-Kader, E.
Nabawy & M. H. Elbana. J. Environ.
Health Sci. Eng., 14 (2016) 15.
https://doi.org/10.1186/s40201-016-0259-6
20. V. T. Pardio, K. N. Waliszewski, L. A.
Landin and R. G. Bautista, Food Addit.
Contam. A, 20 (2003) 259.
https://doi.org/10.1080/0265203021000046
207
21. G. Pagliuca, A. Serraino, T. Gazzotti, E.
Zironi, A. Borsari and R. Rosmini, J.
Dairy Res., 73 (2006) 340.
https://doi.org/10.1017/S002202990600169
5
22. J. Weber, C. J. Halsall, D. Muir, C.
Teixeira, J. Small, K. Solomon and T.
Bidleman, Sci. Total Environ., 408, (2010)
2966.
https://doi.org/10.1016/j.scitotenv.2009.10.
077
23. M. LeDoux, J. Chromatogr. A, 1218,
(2011) 1021.
https://doi.org/10.1016/j.chroma.2010.12.0
97
24. A. Ul Hassan, A. B. Tabinda, M. Abbas
and A. M. Khan, Pak. J. Agri. Sci., 51
(2014) 321.
Pak. J. Anal. Environ. Chem. Vol. 18, No. 1 (2017) 45
25. N. S. Karabasanavar and S. P. Singh, Int. J.
Dairy Technol., 66, (2013) 189.
https://doi.org/10.1111/1471-0307.12007
26. S. Bulut, L. Akkaya, V. Gök and M.
Konuk, Environ. Monit. Assess. 181,
(2011) 555.
https://doi.org/10.1007/s10661-010-1849-x
27. F. Rafael, B. Vanerli, P. P. Ana, D. Karen,
and T. Ronaldo, Pesq. Vet. Bras. 31 (2011)
598.
https://doi.org/10.1590/S0100-
736X2011000700009
28. A. C. Araújo, D. P. Nogueira, and L.G.
Augusto, Revista de Saúde Pública, 34,
(2000) 309.
https://doi.org/10.1590/S0034-
89102000000300016
29. L. A. Nero, M. R. Mattos, V. Beloti, M. A.
F. Barros, D. P. Netto and B. D. G. Franco
de M. Ciênc. Tecnol. Aliment. 27, 201
(2007).
https://doi.org/10.1590/S0101-
20612007000100035
30. E. Kampire, B. T. Kiremire, S. A. Nyanzi
and M. Kishimba, Chemosphere, 84,
(2011) 923.
https://doi.org/10.1016/j.chemosphere.2011
.06.011
31. M. Aslam, S. Rais and M. Alam, J.
Environ. Prot., 4 (2013) 964.
https://doi.org/10.4236/jep.2013.49111
32. B. Schettino, R. Gutiérrez, R. Ortiz, S.
Vega, G. Urban, A. Ramírez, Bull. Environ.
Contam. Toxicol., 91 (2013) 154.
https://doi.org/10.1007/s00128-013-1005-8
33. R. Gutiérrez, S. Vega, R. Ortiz, J. J. Pérez,
and B. Schettino. J. Environ. Sci. Health B.,
50 (2015) 317.
https://doi.org/10.1080/03601234.2015.100
0166
34. M. M. Ayoub, M. E. Desoki, A. S.
Hassanin, W. M. Thabet, M. H. Mansour,
Nagwa M. Loutfy and A. Raslan, J. Plant
Prot. Path., 3 (2012) 865.
35. Da Silva, LCC, V. Beloti, R. Tamanini and
D. P. Netto, Agrarian Sciences,
Londrin., 35 (2014) 2485.
36. K. Kotinagu and N. Krishnaiah, Vet.
World, 8 (2015) 545.
https://doi.org/10.14202/vetworld.2015.545
-550
37. E. M. Shaker and E. E. Elsharkawy,
Environ. Toxicol. Pharmacol., 39 (2015)
433.
https://doi.org/10.1016/j.etap.2014.12.005
38. R. M. Barman, B. K. Mishra and A.
Barman. Int. J. Appl. Pure Sci. Agri. 02
(2016) 1.
39. T. Ismail and W. M. Elkassas, Alexandria
J. Vet. Sci., 48 (2016) 113.
40. F. Muhammad, I. Javed, M. Akhtar, M. M.
Awais, M. K. Saleemi and M. I. Anwar,
Pak. Vet. J., 10 (2012) 4.
41. N. Shahzadi, M. Imran, M. Sarwar, A. S.
Hashmi and M. Wasim, J. Agroaliment.
Proc. Technol., 19 (2013) 167.
42. B. Iftikhar, S. Siddiqui and S. Rehman,
Afr. J. Biotechnol., 13 (2014).
43. A. ul Hassan, A. B. Tabinda, M. Abbas and
A. M. Khan, Pak. J. Agric. Sci., 51 (2014)
321.
44. M. LeDoux, J. Chromatog. A, 1218 (2011)
1021.
