An Innovative Rapid Method for Analysis of 10 Organophosphorus pesticide residues in wheat by HS-SPME-GC-FPD/MSD

Xin Du, Yong Lin Ren, S.J. Beckett

Research output: Contribution to journalArticle

9 Citations (Scopus)

Abstract

The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/ PDMS fiber increased with increasing spiking levels, yielding significant (R2 > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.
Original languageEnglish
Pages (from-to)520-526
Number of pages7
JournalJournal of AOAC International
Volume99
Issue number2
DOIs
Publication statusPublished - 2016

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Pesticide Residues
Solid Phase Microextraction
organophosphorus pesticides
divinyl benzene
pesticide residue
pesticide residues
rapid methods
detectors
Triticum
wheat
Detectors
Fibers
Desorption
desorption
Amber
Mass spectrometers
Pesticides
Linear regression
amber
Food Supply

Cite this

@article{a57da59c85be4118b7ab1c2e90c0eec3,
title = "An Innovative Rapid Method for Analysis of 10 Organophosphorus pesticide residues in wheat by HS-SPME-GC-FPD/MSD",
abstract = "The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/ PDMS fiber increased with increasing spiking levels, yielding significant (R2 > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.",
keywords = "Chemical contamination, Desorption, Extraction, Food supply, Mass spectrometry, Microchannels, Polydimethylsiloxane, Silicones, Spectrometers, Capillary columns, Flame photometric detectors, Headspace solid phase microextraction, Mass spectrometer detectors, Organophos-phorus pesticides, Organophosphorus pesticide, Pesticide residue, Polydimethylsiloxane PDMS, Pesticides",
author = "Xin Du and Ren, {Yong Lin} and S.J. Beckett",
note = "Cited By :2 Export Date: 15 December 2016 CODEN: JAINE Correspondence Address: Ren, Y.L.; Murdoch University, School of Veterinary and Life SciencesAustralia; email: y.ren@murdoch.edu.au References: Johnstone, K., (2006) Queensland University of Technology, , PhD Thesis Australia; (2012) Agricultural and Veterinary Chemicals Code Instrument 4 (MRL Standard), , http://www.comlaw.gov.au/Details/F2014C00970, Australian Pesticides, Veterinary Medicines Authority; Australian Pesticides and Veterinary Medicines Authority, Canberra, Australia; (2008) Official J. Eur. Comm, 9, pp. 67-71. , European Commission Regulation (EC) 299/2008; Ballesteros, E., Parrado, M.D., (2004) J. Chromatogr. A, 1029, pp. 267-273; Anastassiades, M., Lehotay, S.J., Štajnbaher, D., Schenck, F.J., (2003) J. AOAC Int, 86, pp. 412-431; Słowik-Borowiec, M., Szpyrka, E., Walorczyk, S., (2012) Bull. Environ. Contam. Toxicol, 89, pp. 633-637; Lehotay, S.J., De Kok, A., Hiemstra, M., Van Bodegraven, P., (2005) J. AOAC Int, 88, pp. 595-614; D{\'i}ez, C., Traag, W.A., Zommer, P., Marinero, P., Atienza, J., (2006) J. Chromatogr. A, 1131 (11-20); Lehotay, S.J., Mastovsk{\'a}, K., Yun, S.J., (2005) J. AOAC Int, 86, pp. 630-638; Kolberg, D.I., Prestes, O.D., Adaime, M.B., Zanella, R., (2011) Food Chem, 125, pp. 1436-1442; Kataok, H., Lord, H., Pawliszyn, J., (2000) J. Chromatogr. A, 880, pp. 35-62; Pawliszyn, J., Liu, S., (1987) Anal. Chem, 59, pp. 1475-1478; Arthur, C., Pawliszyn, J., (1990) Anal. Chem, 62, pp. 2145-2148; (2014), https://www.sigmaaldrich.com/content/dam/sigma-Aldrich/docs/Supelco/Posters/1/ionic_liquid_gc_columns.pdf, Aldrich Sigma Supelco Introduction, Sigma Aldrich CoBonanse, R.I., Am{\'e}, M.V., Wunderlin, D.A., (2013) Chemosphere, 90, pp. 1860-1869; Doong, R.-A., Liao, P.-L., (2001) J. Chromatogr. A, 918, pp. 177-188; Lambropolou, D.A., Albanis, T.A., (2003) J. Chromatogr. A, 993, pp. 197-203; Yang, K.W., Eisert, R., Lord, H., Pawliszyn, J., (1999) RSC Chromatography Monographs: Applications of Solid Phase Microextraction, pp. 435-477. , J. Pawliszyn (Ed) Royal Society of Chemistry, Cambridge, UK; Fytianos, K., Drimaropoulou, G., Raikos, N., Theodoridis, G., Tsoukali, H.J., (2007) J. AOAC Int, 90, pp. 1677-1681; Ren, Y.L., Padovan, B., Desmarchelier, J.M., (2012) J. AOAC Int, 95, pp. 549-553; Khani, M., Imani, S., Larijan, K., (2011) African J. Food Sci, 5, pp. 499-502; (2007) Official Methods of Analysis, 1. , http://www.eoma.aoac.org/methods/info.asp?ID=48938, AOAC International. Method 2007; (2014) Selection Guide for Supelco SPME Fibres, , http://www.sigmaaldrich.com/analyticalchromatography/sample-preparation/spme/selecting-spme-fiber.html#tips, Sigma Aldrich Co; Kim, D.H., Heo, G.S., Lee, D.W., (1998) J. Chromatogr. A, 824, pp. 63-70",
year = "2016",
doi = "10.5740/jaoacint.15-0062",
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pages = "520--526",
journal = "Journal of the Association of Official Analytical Chemists",
issn = "1060-3271",
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}

An Innovative Rapid Method for Analysis of 10 Organophosphorus pesticide residues in wheat by HS-SPME-GC-FPD/MSD. / Du, Xin; Ren, Yong Lin; Beckett, S.J.

In: Journal of AOAC International, Vol. 99, No. 2, 2016, p. 520-526.

Research output: Contribution to journalArticle

TY - JOUR

T1 - An Innovative Rapid Method for Analysis of 10 Organophosphorus pesticide residues in wheat by HS-SPME-GC-FPD/MSD

AU - Du, Xin

AU - Ren, Yong Lin

AU - Beckett, S.J.

N1 - Cited By :2 Export Date: 15 December 2016 CODEN: JAINE Correspondence Address: Ren, Y.L.; Murdoch University, School of Veterinary and Life SciencesAustralia; email: y.ren@murdoch.edu.au References: Johnstone, K., (2006) Queensland University of Technology, , PhD Thesis Australia; (2012) Agricultural and Veterinary Chemicals Code Instrument 4 (MRL Standard), , http://www.comlaw.gov.au/Details/F2014C00970, Australian Pesticides, Veterinary Medicines Authority; Australian Pesticides and Veterinary Medicines Authority, Canberra, Australia; (2008) Official J. Eur. Comm, 9, pp. 67-71. , European Commission Regulation (EC) 299/2008; Ballesteros, E., Parrado, M.D., (2004) J. Chromatogr. A, 1029, pp. 267-273; Anastassiades, M., Lehotay, S.J., Štajnbaher, D., Schenck, F.J., (2003) J. AOAC Int, 86, pp. 412-431; Słowik-Borowiec, M., Szpyrka, E., Walorczyk, S., (2012) Bull. Environ. Contam. Toxicol, 89, pp. 633-637; Lehotay, S.J., De Kok, A., Hiemstra, M., Van Bodegraven, P., (2005) J. AOAC Int, 88, pp. 595-614; Díez, C., Traag, W.A., Zommer, P., Marinero, P., Atienza, J., (2006) J. Chromatogr. A, 1131 (11-20); Lehotay, S.J., Mastovská, K., Yun, S.J., (2005) J. AOAC Int, 86, pp. 630-638; Kolberg, D.I., Prestes, O.D., Adaime, M.B., Zanella, R., (2011) Food Chem, 125, pp. 1436-1442; Kataok, H., Lord, H., Pawliszyn, J., (2000) J. Chromatogr. A, 880, pp. 35-62; Pawliszyn, J., Liu, S., (1987) Anal. Chem, 59, pp. 1475-1478; Arthur, C., Pawliszyn, J., (1990) Anal. Chem, 62, pp. 2145-2148; (2014), https://www.sigmaaldrich.com/content/dam/sigma-Aldrich/docs/Supelco/Posters/1/ionic_liquid_gc_columns.pdf, Aldrich Sigma Supelco Introduction, Sigma Aldrich CoBonanse, R.I., Amé, M.V., Wunderlin, D.A., (2013) Chemosphere, 90, pp. 1860-1869; Doong, R.-A., Liao, P.-L., (2001) J. Chromatogr. A, 918, pp. 177-188; Lambropolou, D.A., Albanis, T.A., (2003) J. Chromatogr. A, 993, pp. 197-203; Yang, K.W., Eisert, R., Lord, H., Pawliszyn, J., (1999) RSC Chromatography Monographs: Applications of Solid Phase Microextraction, pp. 435-477. , J. Pawliszyn (Ed) Royal Society of Chemistry, Cambridge, UK; Fytianos, K., Drimaropoulou, G., Raikos, N., Theodoridis, G., Tsoukali, H.J., (2007) J. AOAC Int, 90, pp. 1677-1681; Ren, Y.L., Padovan, B., Desmarchelier, J.M., (2012) J. AOAC Int, 95, pp. 549-553; Khani, M., Imani, S., Larijan, K., (2011) African J. Food Sci, 5, pp. 499-502; (2007) Official Methods of Analysis, 1. , http://www.eoma.aoac.org/methods/info.asp?ID=48938, AOAC International. Method 2007; (2014) Selection Guide for Supelco SPME Fibres, , http://www.sigmaaldrich.com/analyticalchromatography/sample-preparation/spme/selecting-spme-fiber.html#tips, Sigma Aldrich Co; Kim, D.H., Heo, G.S., Lee, D.W., (1998) J. Chromatogr. A, 824, pp. 63-70

PY - 2016

Y1 - 2016

N2 - The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/ PDMS fiber increased with increasing spiking levels, yielding significant (R2 > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

AB - The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/ PDMS fiber increased with increasing spiking levels, yielding significant (R2 > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

KW - Chemical contamination

KW - Desorption

KW - Extraction

KW - Food supply

KW - Mass spectrometry

KW - Microchannels

KW - Polydimethylsiloxane

KW - Silicones

KW - Spectrometers

KW - Capillary columns

KW - Flame photometric detectors

KW - Headspace solid phase microextraction

KW - Mass spectrometer detectors

KW - Organophos-phorus pesticides

KW - Organophosphorus pesticide

KW - Pesticide residue

KW - Polydimethylsiloxane PDMS

KW - Pesticides

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UR - http://www.mendeley.com/research/innovative-rapid-method-analysis-10-organophosphorus-pesticide-residues-wheat-hsspmegcfpdmsd

U2 - 10.5740/jaoacint.15-0062

DO - 10.5740/jaoacint.15-0062

M3 - Article

VL - 99

SP - 520

EP - 526

JO - Journal of the Association of Official Analytical Chemists

JF - Journal of the Association of Official Analytical Chemists

SN - 1060-3271

IS - 2

ER -