Abstract
The use of pesticide for the control of insect pests and diseases is increasing day by day. There is a growing concern of health and environmental hazards caused by pesticides and pesticides residues in food and food products. To ensure the supply of safe food, determination of pesticide residues in food and food products plays a key role. At present, different analytical methods are used to determine pesticide residues in food. In this chapter, pesticide residue detection with different analytical techniques, such as: Gas Chromatography (GC), Gas Chromatography Mass Spectrometry (GC-MS), High Performance Liquid Chromatography (HPLC), and Liquid Chromatography Mass Spectrometry (LC-MS) are briefly discussed. Different extraction and clean-up procedures, such as: Liquid-Liquid Extraction (LLE), Super Critical Fluid Extraction (SFE), Solid Phase Extraction (SPE), Solid Phase Micro Extraction (SPME), Stir-bar Sorptive Extraction (SBSE), Microwave-assisted Extraction (MAE) and QuEChERS (Quick, Easy, Cheap, Rugged, and Safe) extraction technique are also presented here.
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Keywords
- High Performance Liquid Chromatography
- Solid Phase Extraction
- Pesticide Residue
- Supercritical Fluid Extraction
- Liquid Chromatography Associate With Mass Spectrometry
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.
1 Introduction
Production of food produces are seriously affected by insect pests and diseases. Due to plant pests and diseases, 20–40% of the crop yields are reduced globally [1]. To overcome these situations farmers are using different kind of pesticides. Pesticides play a key role to control the insect pests and diseases and hence protect and promote production [2]. However, pesticides and pesticide residues in foods may cause several adverse effects on human health and the environment [3,4,5].
Nowadays food safety is a major concern to the consumers [6]. The percentage of food containing pesticide residues has increased in the last 10 years. In order to ensure the supply of safe food, pesticides should be used following Good Agricultural Practices (GAP). Monitoring of pesticide residues in the food is the essential tool to ensure GAP. To monitor pesticide residues in the commercial produces, reliable multi-residue analytical methods are required. Multi-residue analytical methods, which allow the quantification of residues of different analytes simultaneously in a single run, are used advantageously for monitoring purposes. This chapter will briefly discuss different extraction, and analytical detection techniques of pesticides residues in foods.
2 Pesticide Residue Analysis
Concern about pesticide residue analysis is increasing day by day due to the consumers demand for safe food and to serve the trade related obligations [7]. Methods to analyze pesticide residues involve two steps: (a) extraction and clean-up of the target analytes from the matrix, and (b) determination of the target analytes.
2.1 Extraction and Clean-Up
The sample preparation methods to detect pesticide residue in food matrices involve: extraction of target analytes from the bulk of the matrices and partitioning of the residues in an immiscible solvent, and/or clean-up of the analytes from the matrix co-.extractives. Complex samples like meat and meat products require two step clean-up which combines different chromatographic techniques [8].
Different techniques are used to extract and clean-up of pesticides from different food matrices, such as: liquid-liquid extraction (LLE), super critical fluid extraction (SFE), microwave-assisted extraction (MAE), solid phase extraction (SPE), solid phase micro extraction (SPME), stir-bar sorptive extraction (SBSE), and QuEChERS extraction etc.
2.1.1 Liquid–Liquid Extraction (LLE)
Liquid–liquid extraction is an important separation technique, which is also known as solvent extraction and partitioning. It is widely used in the modern process industry and it is a basic technique in the chemical laboratories. This extraction technique is mainly based on different degrees of solubility of components in two immiscible, or partially miscible, liquids. It is a separation technique of a substance from one liquid into another liquid phase. Both of the liquids are thoroughly contacted and subsequently separated from each other again.
2.1.2 Supercritical Fluid Extraction (SFE)
Supercritical fluid extraction is a technique where supercritical fluids are used as the extracting solvent to separate one component or to separate desired analytes (pesticides) from the matrix. Usually CO2 is used as a supercritical fluid. This technique is more effective for the solid matrix but it can also be used to separate desired analyte from the liquid matrix. This extraction process is used for analytical purposes to extract the analytes from the matrix, and to strip unwanted material from a product (decaffeination) or collect a desired product (e.g. essential oils).
2.1.3 Solid-Phase Extraction (SPE)
Solid phase extraction (SPE) is a rapid, reliable, and selective sample preparation technique. Solid phase extraction technique is used to extract the analytes from different matrices such as urine, blood, water, beverages, soil, and animal tissue [9]. In the analytical laboratories, this extraction technique is used to concentrate and purify samples for analysis using HPLC, GC, GC-MS and LC-MS/MS. It extends the lifetime of chromatographic systems and improves the qualitative and quantitative analysis.
2.1.4 Solid-phase microextraction (SPME)
Solid-phase microextraction is a fast, solvent-free extraction technique that involves the use of a fiber coated with an extracting phase, which can be a liquid or a solid [10]. Different kinds of analytes including volatile and non-volatile compounds from different kinds of media are extracted by this extraction technique [11]. SPME is compatible with analyte separation/detection by GC or HPLC, and provides a very good result for wide concentrations of analytes.
2.1.5 Stir Bar Sorptive Extraction (SBSE)
Stir-bar sorptive extraction (SBSE) belongs to a group of techniques which was first developed for sampling in liquid phase and is based upon sorption of the investigated analytes or fraction onto a very thick film of PDMS coated onto a glass-coated magnetic stir bar (commercially known as Twister, Gerstel GmbH, Muelheim, Germany).
2.1.6 Microwave-Assisted Extraction (MAE)
Microwave-assisted extraction is an efficient method that involves deriving natural compounds from raw plants. MAE technique allows organic compounds to be extracted more rapidly, with similar or better yield as compared to conventional extraction methods.
2.1.7 QuEChERS Extraction
One of the latest extraction and clean-up techniques for pesticide residue analysis in food matrices is the QuEChERS (quick, easy, cheap, effective, rugged and safe) technique, which was first introduced by Anastassiades et al. [12] in 2003. QuEChERS employs a novel and much quicker dispersive solid phase extraction (dSPE) cleanup. This technique was modified by several research groups (AOAC Official methods, 2007.1; the European Committee for Standardization (CSN) Standard Method, CSN EN 15662, 2008) [13, 14]. Because of high analyte recoveries, the low organic solvent consumption, and the low cost per sample, QuEChERS technique is gradually gaining popularity compared to other existing technique.
At present QuEChERS technique is widely used for the extraction and clean-up of the extracts of fruit and vegetable matrices [1, 15,16,17,18,19,20,21,22,23,24,25,26,27,28,29,30,31,32,33,34,35,36,37,38,39,40], dairy and fatty matrices [41,42,43,44], matrices of grains, nuts and seeds [38, 45,46,47,48,49], and matrices of baby foods [50,51,52,53,54,55,56,57,58,59,60].
2.2 Pesticide Residue Determination
Gas Chromatography (GC), Gas Chromatography associated with Mass Spectrometry (GCMS), High Performance Liquid Chromatography (HPLC), and Liquid Chromatography associated with Mass Spectrometry (LC-MS) are the most commonly used techniques to detect pesticides and pesticide residues in foods.
2.2.1 Gas Chromatography (GC)
A gas chromatograph (GC) is an analytical instrument that measures the content of various components in a sample. There are different detectors, with different types of selectivity, can be used in gas chromatography. Flame ionization detector (FID) is feasible for most of the organic compounds. Thermal conductivity detector (TCD) is a universal detector. Electron capture detector (ECD) is used for halides, nitrates, nitriles, peroxides, anhydrides, organometallics etc. Nitrogen-phosphorus detector (NPD) is normally used for nitrogen, phosphorus and the Flame photometric detector (FPD) is used for sulphur, phosphorus, tin, boron, arsenic, germanium, selenium and chromium. Till date, GC technique with different detectors are used for the quantification of pesticide residues from different food matrices [81, 87,88,89,90,91,92,93,94].
2.2.2 Gas Chromatography–Mass Spectrometry (GC–MS)
In GC-MS, pesticides are identified by retention time and specific ions, and quantified by selected ion monitoring (SIM) mode using the target and qualified ions. SIM mode provides adequate quantification at low concentration. However, the accuracy may be reduced if the selected ions are affected by matrix effect. Besides using the MS/MS it is possible to decrease the matrix effects, may achieve a higher selectivity levels and lower detection limit [51, 76]. GC-MS/MS with triple quadrupole [76, 77] and ion trap mass spectrometers [77] has been used for pesticide residue analysis on fatty food. To analyze multiple pesticide residues from food matrices using GC-MS, acquisition mode, multiple reaction monitoring (MRM) [76], and the selected reaction monitoring (SRM) [78] mode have been used. Several single and multiresidue methods using GC-MS have been developed for the analysis of pesticides from different classes [79,80,81,82,83,84,85,86,87,88].
2.2.3 Liquid Chromatography-Mass Spectrometry (LC-MS)
In recent years, LC-MS has been used to determine pesticide residues in fruit and vegetable extract. LC-MS is an effective technique that generally reduces the excessive clean-up steps, exhibits little chance of false-positive findings, and reduces the analysis time and cost [61]. The high sensitivity of LC-MS technique makes it useful in many applications. Different mass analyzers are used in LC-MS, including single quadrupole, triple quadrupole, ion trap, and time of flight mass spectrometry (TOF-MS). LC-MS/MS with electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) source are used widely to analyze multiple pesticide residues from a wide variety of matrices [2, 21, 62,63,64,65,66,67,68,69,70,71,73]. A wide range of pesticides can be analysed by both GC-MS and LC-MS techniques. However, LC-MS is considered to cover a wider scope than GC-MS [74]. LC-MS/MS with ESI (electrospray ionization) and APCI (atmospheric pressure chemical ionization) source have improved the feasibility of the identification of pesticides of different chemical structures in food at concentrations comparable to those obtained by GC-MS [75].
2.2.4 High Performance Liquid Chromatography (HPLC)
High Performance Liquid Chromatography (HPLC) has been used for manufacturing (e.g. during the production process of pharmaceutical and biological products), legal (e.g. detecting performance enhancement drugs in urine), research (e.g. separating the components of a complex biological sample, or of similar synthetic chemicals from each other), and medical (e.g. detecting vitamin D levels in blood serum) purposes. Nowadays, HPLC is mostly used for the purity analysis of pesticides. It is also used for single pesticide residue analysis of different food matrices [15, 89].
The commonly used detectors for pesticide residue analysis are UV-VIS Detector, Photo Diode Array Detector (PDA) and Fluorescence Detector. UV-VIS Detector is the most commonly used detector. The response of UV-VIS Detector is specific to a particular compound or class of compounds depending on the presence of light absorbing functional groups of eluting molecules. Fluorescence detector gives higher sensitivity than a UV-VIS detector. Photo Diode Array Detector (PDA) helps to monitor simultaneous determination of more than one absorbing component at different wavelengths.
3 Conclusion
Analytical methods discussed in this chapter play an important role for the qualitative and quantitative detection of pesticide residues in food matrices. Prior to analyze the sample, the analytical methods should be validated in terms of accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity [95].
References
FAO, Global pact against plant pests marks 60 years in action. FAO celebrates anniversary of creation of the International Plant Protection Convention in 3 April 2012, Rome (2012), http://www.fao.org/news/story/en/item/131114/icode/
M.D.H. Prodhan, E.N. Papadakis, E. Papadopoulou-Mourkidou, Analysis of pesticide residues in melon using QuEChERS extraction and liquid chromatography triple quadrupole mass spectrometry. Int. J. Environ. Anal. Chem. (2015) http://dx.doi.org/10.1080/03067319.2015.1025227
J. Fenik, M. Tankiewicz, M. Biziuk, Properties and determination of pesticides in fruits and vegetables. Trends Anal. Chem. 30(6), 814–826 (2011)
A.N. McIntyre, N. Allision, D.R. Penman, Pesticides: Issues and Options for New Zealand (Ministry for the Environment, Wellington, 1989)
J. Hajslova, J. Zrostlikova, Matrix effects in (ultra)trace analysis of pesticide residues in food and biotic matrices. J. Chrom. A 1000(1–2), 181–197 (2003)
Pesticide Action Network (PAN), Europe. European food is not safe as European Food Safety authority pretends (2014), www.pan-europe.info/news/PR/140522.html
Z. Parveen, I.S. Riazuddin, M.I. Khuhro, M.A. Bhutto, M. Ahmed, Monitoring of multiple pesticide residues in some fruits in Karachi. Pakistan. Pak. J. Bot. 43(4), 1915–1918 (2011)
G.G. Rimkus, M. Rummler, I. Nausch, Gel permeation chromatography-high performance liquid chromatography combination as an automated clean-up technique for the multiresidue analysis of fats. J. Chromatogr. A 737(1), 9–14 (1996)
H. Marie-Claire, Solid-phase extraction: method development, sorbents, and coupling with liquid chromatography. J. Chromatogr. A 856(1–2), 3–54 (1999). doi:10.1016/S0021-9673(99)00832-8. ISSN 0021-9673
A. Spietelun, M. Pilarczyk, A. Kloskowski, J. Namieśnik, Current trends in solid-phase microextraction (SPME) fibre coatings. Chem. Soc. Rev. 39(11), 4524 (2010). doi:10.1039/c003335a. ISSN 0306-0012
S. Mitra, Sample Preparation Techniques in Analytical Chemistry (Jon, Hoboken, 2003), p. 113
M. Anastassiades, S.J. Lehotay, D. Stajnbaher, F.J. Schenck, Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J. AOAC Int. 86, 412–431 (2003)
AOAC Official Method 2007.01. Pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate
CSN EN 15662, Foods of plant origin- determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE- QuEChERS method (2008), www.en-standard.eu/15562
M. Paramasivam, S. Chandrasekaran, Determination of fipronil and its major metabolites in vegetables, fruit and soil using QuEChERS and gas chromatography-mass spectrometry. Int. J. Environ. Anal. Chem. 93(11), 1203–1211 (2012)
B. Gilbert-Lopez, F. Juan Garcia-Reyes, A. Lozano, A.R. Fernandez-Alba, A. Molina-Diaz, Large-scale pesticide testing in olives by liquid chromatography–electrospray tandem mass spectrometry using two sample preparation methods based on matrix solid-phase dispersion and QuEChERS. J. Chromatogr. A 1217, 6022–6035 (2010)
S.J. Lehotay, A.S. Kyung, H. Kwon, U. Koesukwiwat, W. Fu, K. Mastovska, E. Hoh, N. Leepipatpiboon, Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J. Chromatogr. A 1217, 2548–2560 (2010)
S.J. Lehotay, A. De Kok, M. Hiemstra, B.P. Van, Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection. J. AOAC Int. 88(2), 595–614 (2005)
S.J. Lehotay, Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. J. AOAC Int. 90(2), 485–520 (2007)
B. Singh, A. Kar, K. Mandal, R. Kumar, S.K. Sahoo, Development and validation of QuEChERS method for estimation of chlorantraniliprole residue in vegetables. J. Food Sci. 77(12), T208–T215 (2012). doi:10.1111/j.1750-3841.2012.02801.x
R. Dasika, S. Tangirala, P. Naishadham, Pesticide residue analysis of fruits and vegetables. J Environ. Chem. Ecotoxicol. 4(2), 19–28 (2012)
N. Mantzos, A. Karakitsou, I. Zioris, E. Leneti, I. Konstantinou, QuECHERS and soil phase extraction methods for the determination of energy crop pesticides in soil, plantand runoff water matrices. Int. J. Environ. Anal. Chem. 93(15), 1566–1584 (2013)
M.R. Kirchner, E. Húsková, J.M. Matisová, Fast gas chromatography for pesticide residues analysis using analyte protectants. J. Chromatogr. A 1186, 271–280 (2008)
K. Banerjee, D.P. Oulkar, S.B. Patil, M.R. Jadhav, S. Dasgupta, S.H. Patil, S. Bal, P.G. Adsule, Multiresidue determination and uncertainty analysis of 87 pesticides in mango by liquid chromatography-tandem mass spectrometry. J. Agric. Food Chem. 57(10), 4068–4078 (2009). doi:10.1021/jf900358r. Epub 2009 Apr 20
F.J. Schenck, A.N. Brown, L.V. Podhorniak, A. Parker, M. Reliford, J.W. Wong, A rapid multiresidue method for determination of pesticides in fruits and vegetables by using acetonitrile extraction/partitioning and solid-phase extraction column cleanup. J. AOAC Int. 91(2), 422–438 (2008)
T. Kovalczuk, O. Lacina, M. Jech, J. Poustka, J. Hajslová, Novel approach to fast determination of multiple pesticide residues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Food Addit. Contam. Part A 25(4), 444–457 (2008). doi:10.1080/02652030701570156
R. Romero-GonzAlez, A. Garrido Frenich, J.L. Martínez Vidal, Multiresidue method for fast determination of pesticides in fruit juices by ultra performance liquid chromatography coupled to tandem mass spectrometry. Talanta 76(1), 211–225 (2008). doi:10.1016/j.talanta.2008.02.041
B. Kmellár, P. Fodor, L. Pareja, C. Ferrer, M.A. Martínez-Uroz, A. Valverde, A.R. Fernandez-Alba, Validation and uncertainty study of a comprehensive list of 160 pesticide residues in multi-class vegetables by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1215(1–2), 37–50 (2008). doi:10.1016/j.chroma.2008.10.121
S.C. Cunha, S.J. Lehotay, K. Mastovska, J.O. Fernandes, M. Beatriz, P.P. Oliveira, Evaluation of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives. J. Sep. Sci. 30(4), 620–632 (2007)
L. Li, W. Li, D. Qin, S. Jiang, F. Liu, Application of graphitized carbon black to the QuEChERS method for pesticide multiresidue analysis in spinach. J. AOAC Int. 92(2), 538–547 (2009)
F. Schenck, J. Wong, C. Lu, J. Li, J.R. Holcomb, L.M. Mitchell, Multiresidue analysis of 102 organophosphorus pesticides in produce at parts-per-billion levels using a modified QuEChERS method and gas chromatography with pulsed flame photometric detection. J. AOAC Int. 92(2), 561–573 (2009)
R. Húsková, E. Matisová, L. Svorc, J. Mocák, M. Kirchner, Comparison of negative chemical ionization and electron impact ionization in gas chromatography-mass spectrometry of endocrine disrupting pesticides. J. Chromatogr. A 1216(24), 4927–4932 (2009). doi:10.1016/j.chroma.2009.04.045
H.G. Mol, A. Rooseboom, R. van Dam, M. Roding, K. Arondeus, S. Sunarto, Modification and re-validation of the ethyl acetate-based multi-residue method for pesticides in produce. Anal. Bioanal. Chem. 389(6), 1715–1754 (2007)
F. Ji, L. Zhao, W. Yan, Q. Feng, J.M. Lin, Determination of triazine herbicides in fruits and vegetables using dispersive solid-phase extraction coupled with LC-MS. J. Sep. Sci. 31(6–7), 961–968 (2008). doi:10.1002/jssc.200700610
M. Mezcua, C. Ferrer, J.F. García-Reyes, M.J. Martínez-Bueno, M. Albarracín, M. Claret, A.R. Fernández-Alba, Determination of selected non-authorized insecticides in peppers by liquid chromatography time-of-flight mass spectrometry and tandem mass spectrometry. Rapid Commun. Mass Spectrom. 22(9), 1384–1392 (2008). doi:10.1002/rcm.3515
J.L. Fernández Moreno, A. Garrido Frenich, P. Plaza Bolaños, J.L. Martínez Vidal, Multiresidue method for the analysis of more than 140 pesticide residues in fruits and vegetables by gas chromatography coupled to triple quadrupole mass spectrometry. J. Mass Spectrom. 43(9), 1235–1254 (2008). doi:10.1002/jms.1400
K. Banerjee, D.P. Oulkar, S.B. Patil, S.H. Patil, S. Dasgupta, R. Savant, P.G. Adsule, Single-laboratory validation and uncertainty analysis of 82 pesticides determined in pomegranate, apple, and orange by ethyl acetate extraction and liquid chromatography/tandem mass spectrometry. J. AOAC Int. 91(6), 1435–1445 (2008)
S. Walorczyk, Application of gas chromatography/tandem quadrupole mass spectrometry to the multi-residue analysis of pesticides in green leafy vegetables. Rapid Commun. Mass Spectrom. 22(23), 3791–3801 (2008). doi:10.1002/rcm.3800
K. Zhang, J.W. Wong, D.G. Hayward, P. Sheladia, A.J. Krynitsky, F.J. Schenck, M.G. Webster, J.A. Ammann, S.E. Ebeler, Multiresidue pesticide analysis of wines by dispersive solid-phase extraction and ultrahigh-performance liquid chromatography-tandem mass spectrometry. J. Agric. Food Chem. 57(10), 4019–4029 (2009). doi:10.1021/jf9000023
K. Banerjee, D.P. Oulkar, S. Dasgupta, S.B. Patil, S.H. Patil, R. Savant, P.G. Adsule, Validation and uncertainty analysis of a multi-residue method for pesticides in grapes using ethyl acetate extraction and liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1173(1–2), 98–109 (2007)
S.C. Cunha, J.O. Fernandes, A. Alves, M.B. Oliveira, Fast low-pressure gas chromatography-mass spectrometry method for the determination of multiple pesticides in grapes, musts and wines. J. Chromatogr. A 1216(1), 119–126 (2009). doi:10.1016/j.chroma.2008.11.015
S.J. Lehotay, K. Mastovská, S.J. Yun, Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes. J. AOAC Int. L. 88(2), 630–638 (2005)
M.M. Aguilera-Luiz, J.L. Vidal, R. Romero-González, A.G. Frenich, Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry. J. Chromatogr. A 1205(1–2), 10–16 (2008). doi:10.1016/j.chroma.2008.07.066
T. Dagnac, M. Garcia-Chao, P. Pulleiro, C. Garcia-Jares, M. Llompart, Dispersive solid-phase extraction followed by liquid chromatography-tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk. J. Chromatogr. A 1216(18), 3702–3709 (2009). doi:10.1016/j.chroma.2009.02.048
C. Diez, W.A. Traag, P. Zommer, P. Marinero, J. Atienza, Comparison of an acetonitrile extraction/partitioning and “dispersive solid-phase extraction” method with classical multi-residue methods for the extraction of herbicide residues in barley samples. J. Chromatogr. A 1131(1–2), 11–23 (2006)
T.D. Nguyen, B.S. Lee, B.R. Lee, D.M. Lee, G.H. Lee, A multiresidue method for the determination of 109 pesticides in rice using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography/mass spectrometry with temperature control and vacuum concentration. Rapid Commun. Mass Spectrom. 21(18), 3115–3122 (2007)
T.D. Nguyen, E.M. Han, M.S. Seo, S.R. Kim, M.Y. Yun, D.M. Lee, G.H. Lee, A multi-residue method for the determination of 203 pesticides in rice paddies using gas chromatography/mass spectrometry. Anal. Chim. Acta 619(1), 67–74 (2008). doi:10.1016/j.aca.2008.03.031
U. Koesukwiwat, K. Sanguankaew, N. Leepipatpiboon, Rapid determination of phenoxy acid residues in rice by modified QuEChERS extraction and liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta 626(1), 10–20 (2008). doi:10.1016/j.aca.2008.07.034
M.K. Van der Lee, G. van der Weg, W.A. Traag, H.G. Mol, Qualitative screening and quantitative determination of pesticides and contaminants in animal feed using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry. J. Chromatogr. A 1186(1–2), 325–339 (2008)
A. Hercegová, M. Dömötörová, E. Matisová, Sample preparation methods in the analysis of pesticide residues in baby food with subsequent chromatographic determination. J. Chromatogr. A 1153 (1–2, 54–73 (2007)
T. Cajka, J. Hajslova, O. Lacina, K. Mastovska, S.J. Lehotay, Rapid analysis of multiple pesticide residues in fruit-based baby food using programmed temperature vaporiser injection-low-pressure gas chromatography-high-resolution time-of-flight mass spectrometry. J. Chromatogr. A 1186(1–2), 281–294 (2008). doi:10.1016/j.chroma.2007.12.009. Epub 2007 Dec 8
J. Wang, D. Leung, Determination of 142 pesticides in fruit- and vegetable-based infant foods by liquid chromatography/electrospray ionization-tandem mass spectrometry and estimation of measurement uncertainty. J. AOAC Int. 92(1), 279–301 (2009)
J. Wang, D. Leung, Applications of ultra-performance liquid chromatography electrospray ionization quadrupole time-of-flight mass spectrometry on analysis of 138 pesticides in fruit- and vegetable-based infant foods. J. Agric. Food Chem. 57(6), 2162–2173. doi:10.1021/jf803419j
C. Przybylski, C. Segard, Method for routine screening of pesticides and metabolites in meat based baby-food using extraction and gas chromatography-mass spectrometry. J. Sep. Sci. 32(11), 1858–1867 (2009). doi:10.1002/jssc.200900016
C.L. Cristiana, H. Peter, R.J. Fussell, B.J. Keely, Comparison of ultra-performance liquid chromatography and high-performance liquid chromatography for the determination of priority pesticides in baby foods by tandem quadrupole mass spectrometry. J. Chromatogr. A 1103(1, 94–101 (2006)
C.L. Cristiana, R.J. Fussell, B.J. Keely, Determination of priority pesticides in baby foods by gas chromatography tandem quadrupole mass spectrometry. J. Chromatogr. A 1085(2, 207–212 (2005)
B. Gilbert-López, J.F. García-Reyes, P. Ortega-Barrales, A. Molina-Díaz, A.R. Fernández-Alba, Analyses of pesticide residues in fruit-based baby food by liquid chromatography/electrospray ionization time-of-flight mass spectrometry. Rapid Commun. Mass Spectrom. 21(13), 2059–2071 (2007)
C.C. Leandro, P. Hancock, R.J. Fussell, B.J. Keely, Ultra-performance liquid chromatography for the determination of pesticide residues in foods by tandem quadrupole mass spectrometry with polarity switching. J. Chromatogr. A 1144(2), 161–169 (2007)
C.C. Leandro, P. Hancock, R.J. Fussell, B.J. Keely, Quantification and screening of pesticide residues in food by gas chromatography-exact mass time-of-flight mass spectrometry. J. Chromatogr. A 1166(1–2), 152–162 (2007)
A. Hercegová, M. Dömötörová, D. Kruzlicová, E. Matisová, Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry for ultratrace analysis of pesticide residues in baby food. J. Sep. Sci. 29(8), 1102–1109 (2006)
M. Heimstra, A. de Kok, Comprehensive multi-residue method for the target analysis of pesticides in crops using liquid chromatography–tandem mass spectrometry. J. Chromatogr. A 1154, 3–25 (2007)
M.D.H. Prodhan, E.N. Papadakis, E. Papadopoulou-Mourkidou, Determination of multiple pesticide residues in eggplant with Liquid Chromatography – Mass Spectrometry. Food Anal. Methods 8, 229–235 (2015)
A. Garrido Frenich, J.L. Martinez Vidal, T. Lopez Lopez, S.C. Aquado, S.I. Martinez, Monitoring multiclass pesticide residues in fresh fruits and vegetables by liquid chromatography with tandem mass spectrometry. J. Chromatogr. A 1048, 199–206 (2004)
F.J. Camino-Sancheza, A. Zafra-Gomez, B. Oliver-Rodriguezb, O. Ballesteros, A. Navalon, G. Crovetto, J.L. Vilchez, UNE-EN ISO/IEC 17025:2005-accredited method for the determination of pesticide residues in fruit and vegetable samples by LC-MS/MS. Food Addit. Contam. 27(11), 1532–1544 (2010)
P. Caboni, G. Sarais, A. Angioni, S. Vargiu, D. Pagnozzi, P. Cabras, J.E. Casida, Liquid chromatography tandem mass spectrometric ion switching determination of chlorantraniliprole and flubendiamide in fruits and vegetables. J. Agric. Food Chem. 56, 7696–7699 (2008)
H. Obana, M. Okihashi, K. Akutsu, Y. Kitagawa, S. Hori, Determination of neonicotinoid pesticide residues in vegetables and fruits with Solid Phase Extraction and Liquid Chromatography Mass Spectrometry. J. Agric. Food Chem. 51, 2501–2505 (2003)
C. Jansson, T. Pihlström, B.-G. Österdahl, K.E. Markides, A new multi-residue method for analysis of pesticide residues in fruit and vegetables using liquid chromatography with tandem mass spectrometric detection. J. Chromatogr. A 1023, 93–104 (2004)
I. Ferrer, J.F. Garcia-Reyes, M. Mezcua, E.M. Thurman, A.R. Fernandez-Alba, Multi-residue pesticide analysis in fruits and vegetables by liquid chromatography–time-of-flight mass spectrometry. J. Chromatogr. A 1082(1), 81–90 (2005)
L. Lucini, G.P. Molinari, Performance and matrix effect observed in QuEChERS extraction and tandem mass spectrometry analyses of pesticide residues in different target crops. J Chromatogr. Sci. 49, 709–714 (2011)
T. Satoshi, H. Yamamoto, N. Fukui, S. Yamaguchi, Y. Kitagawa, Y. Kakimoto, M. Osakada, M. Okihashi, K. Kajimura, H. Obana, Validation study on a rapid multi-residue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS. Food Hyg. Saf. Sci. 54(3), 237–249 (2013)
G.F. Pang, C.L. Fan, Y.M. Liu, Y.Z. Cao, J.J. Zhang, X.M. Li, Z.Y. Li, Y.P. Wu, T.T. Guo, Determination of residues of 446 pesticides in fruits and vegetables by three-cartridge solid-phase extraction-gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. J. AOAC Int. 89(3), 740–771 (2006)
H.G. Mol, R.C. van Dam, O.M. Steijger, Determination of polar organophosphorus pesticides in vegetables and fruits using liquid chromatography with tandem mass spectrometry: selection of extraction solvent. J. Chromatogr. A 1015, 119–127 (2003)
S. Fan, P. Zhao, C. Yu, C. Pan, X. Li, Simultaneous determination of 36 pesticide residues in spinach and cauliflower by LC-MS/MS using multiwalled carbon nanotubes-based dispersive solid-phase clean-up. Food Addit. Contam. Part A 31(1), 73–82 (2014)
H.G.J. Mol, P. Plaza- Bolanos, P. Zomer, T.C. De Rijk, S. AAM, M. PPJ, Toward a generic extraction method for simultaneous determination of pesticides, mycotoxins, plant toxins and veterinary drugs in feed and food matrixes. Anal. Chem. 80, 9450–9459 (2008)
Y. Pico, G. Font, M.J. Ruiz, M. Fernandez, Control of pesticide residues by liquid chromatography-mass spectrometry to ensure food safety. Mass Spectrom. Rev. 25, 917–960 (2006)
K. Patel, R.J. Fussel, M. Hetmanski, D.M. Goodall, B.J. Keely, Evaluation of gas chromatography–tandem quadrupole mass spectrometry for the determination of organochlorine pesticides in fats and oils. J. Chromatogr. A 1068, 289–296 (2005)
D. Wang, S. Atkinson, A. Hoover-Miller, Q.X. Li, Analysis of organochlorines in harbor seal (Phoca vitulina) tissue samples from Alaska using gas chromatography/ion trap mass spectrometry by an isotopic dilution technique. Rapid Commun. Mass Spectrom. 19, 1815–1821 (2005)
A. Garrido Frenich, J.L. Martinez Vidal, A.D. Cruz Sicilia, M.J. Gonzalez Rodriguez, B. Plaza, Multiresidue analysis of organochlorine and organophosphorus pesticides in muscle of chicken, pork and lamb by gas chromatography-triple quadrupole mass spectrometry. Anal. Chim. Acta 558, 42–52 (2006)
A. Garrido Frenich, J.L. Martinez Vidal, M. Moreno Frias, F. Olea-Serrano, N. Olea, L. Cuadros-Rodreguez, Determination of organochlorine pesticides by GC-ECD and GC-MS-MS techniques including an evaluation of the uncertainty associated with the results. Chromatographia 5, 213–220 (2003)
H. Akhlaghi, A. Motavalizadehkakhky, R. Emamiyan, Determination of diazinon in fruits from northeast of Iran using the QuEChERS sample Ppeparation method and GC/MS. Asian J. Chem. 25(3), 1727–1729 (2013)
Y. Latif, S.T.H. Sherazi, M.I. Bhanger, Assessment of pesticide residues in commonly used vegetables in Hyderabad, Pakistan. Ecotoxicol. Environ. Saf. 74, 2299–2303 (2011)
M.H. El-Saeid, M.T. Selim, Multiresidue analysis of 86 pesticides using gas chromatography mass spectrometry: ii-nonleafy vegetables. J. Chem. 10 pages, Article ID 727149 (2013), http://dx.doi.org/10.1155/2013/727149
S.S. Chauhan, S. Negi, N. Singh, G. Bhatia, A. Srivastava, Monitoring of pesticides residues in farmgate vegetables of Uttarakhand, India. Wudpecker J. Agric. Res. 1(7), 250–256 (2012)
Z. Hadian, M.H. Azizi, H. Hosseiny, K. Khosravi-darani, Determination of pesticides in fruits by gas chromatography/mass spectrometry after high performance gel permeation clean up. Asian J. Chem. 20(4), 2643–2650 (2008)
S. Chandra, A.N. Mahindrakar, L.P. Shinde, Capillary gas chromatography-mass spectrometry determination of pesticide residues in vegetables. Middle-East J. Sci. Res. 11(5), 589–594 (2012)
R. Paranthaman, A. Sudha, S. Kumaravel, Determination of pesticide residues in banana by using high performance liquid chromatography and gas chromatography-mass spectrometry. Am. J. Biochem. Biotechnol. 8(1), 1–6 (2012)
J.L.M. Vidal, F.J. Arrebola, A. Garrido Frenich, J.M. Fernandez, M. Mateu-Sanchez, Validation of a gas chromatographic– tandem mass spectrometric method for analysis of pesticide residues in six food commodities. selection of a reference matrix for calibration. Chromatographia 59, 321–327 (2004)
K.H. Kabir, M. Abdullah, M.D.H. Prodhan, M.S. Ahmed, M.N. Alam, Determination of carbofuran residue in the samples of sugarcane and soil of sugarcane field. Agriculturist 5(1& 2), 61–66 (2007)
A.A. Panhwar, A.S. Saghir, Assessment of pesticide residues in cauliflower through gas chromatography-μECD and high performance liquid chromatography (HPLC) analysis. Int. J. Agric. Sci. Res. 3(1), 7–16 (2013)
C.K. Bempah, A. Buah-Kwofie, D. Denutsui, J. Asomaning, A.O. Tutu, Monitoring of pesticide residues in fruits and vegetables and related health risk assessment in Kumasi Metropolis, Ghana. Res. J. Environ. Earth Sci. 3(6), 761–771 (2011)
A.K. Srivastava, P. Trivedi, M.K. Srivastava, M. Lohani, L.P. Srivastava, Monitoring of pesticide residues in market basket samples of vegetable from Lucknow City, India: QuEChERS method. Environ. Monit. Assess. 176, 465–472 (2011)
S. Chandra, A.N. Mahindrakar, L.P. Shinde, Determination of cypermethrin and chlorpyrifos in vegetables by GC-ECD. Int. J. ChemTech Res CODEN( USA) IJCRGG 2(2), 908–911 (2010)
K.H. Kabir, M.A. Rahman, M.S. Ahmed, M.D.H. Prodhan, M.W. Akon, Determination of residue of diazinon and carbosulfan in brinjal and quinalphos in yard long bean under supervised field trial. Bangladesh J. Agric. Res. 33(3), 503–513 (2008)
J. Hajslova, K. Holadova, V. Kocourek, J. Poustka, M. Godula, P. Cuhra, M. Kempny, Matrix-induced effects: a critical point in the gas chromatographic analysis of pesticide residues. J. Chromatogr. A 800, 283–295 (1998)
European Commission, Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. Document no. SANCO/12571/2013 (2013)
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Prodhan, M.D.H., Alam, S.N., Jalal Uddin, M. (2017). Analytical Methods in Measuring Pesticides in Foods. In: Khan, M., Rahman, M. (eds) Pesticide Residue in Foods. Springer, Cham. https://doi.org/10.1007/978-3-319-52683-6_8
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