Skip to main content
SpringerLink
Log in

Trace Analysis of Fluroxypyr-Meptyl and Fluroxypyr in Wheat and Soil Ecosystem Based on Ion Column-Solid Phase Extraction Method and Liquid Chromatography-Tandem Mass Spectrometry

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

The study developed a novel purification procedure with ion column-solid-phase extraction (IC-SPE) for analysis of fluroxypyr-meptyl and fluroxypyr in wheat samples by liquid chromatography tandem mass spectrometry. During the sample preparation, IC-SPE method was carried out with the column containing the selection of adsorbent materials and with the help of syringes to pull and push extract through adsorbents. Based on a modified quick, easy, cheap, effective, rugged, and safe sample preparation, the ratio of water (containing 0.1% formic acid) to extraction solvent, cleanup adsorbents, and IC-SPE cycle times was studied for analyzing the residues in wheat grain, seedling, straw, and soil. The mean recoveries ranged from 82 to 107% with relative standard deviations below 10% for all matrices. Good linearity was obtained at the range of 0.005~1.0 mg L−1 for the analytes in the selected matrices. The limit of quantification for target analytes was between 0.05 and 0.1 mg kg−1. A field trial including dissipation kinetics and terminal residue study was conducted under open field conditions at three sites during the year of 2015–2016 to monitor the residue level of fluroxypyr-meptyl and fluroxypyr in wheat and soil samples. The results suggested that the developed method was successfully applied to the routine monitoring of fluroxypyr-meptyl or fluroxypyr residues in practical samples.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

Abbreviations

IC-SPE:

Ion column solid phase extraction

MRL:

Maximum residue limit

dSPE:

Dispersive solid phase extraction

PSA:

Primary secondary amine

GCB:

Graphitized carbon black

C18:

Octadecyl silica

MWCNT:

Multi walled carbon nanotube

LC-MS/MS:

Liquid chromatography-tandem mass spectrometry

ESI:

Electrospray ionization

MRM:

Multiple reaction monitoring

CE:

Collision energy

RSD:

Relative standard deviation

ME:

Matrix effect

References

  • Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) 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

    CAS  PubMed  Google Scholar 

  • Bjorling-Poulsen M, Andersen HR, Grandjean P (2008) Potential developmental neurotoxicity of pesticides used in Europe. Environ Health 7:1–22

    Article  CAS  Google Scholar 

  • Bolaños PP, Frenich AG, Vidal JM (2007) Application of gas chromatography-triple quadrupole mass spectrometry in the quantification-confirmation of pesticides and polychlorinated biphenyls in eggs at trace levels. J Chromatogr A 1167:9–17

    Article  CAS  PubMed  Google Scholar 

  • Bruzzoniti MC, Checchini L, De Carlo RM, Orlandini S, Rivoira L, Del Bubba M (2014) QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices, a critical review. Anal Bioanal Chem 406:4089–4116

    Article  CAS  PubMed  Google Scholar 

  • Curtis BC, Rajaram S, Macpherson HG (2002) Bread wheat–improvement and production. Rome, Food and Agriculture Organization of the United Nations

  • EPA (1998) Fluroxypyr Fact sheet, http, //www.epa.gov/opprd001/factsheets/fluroxypyr.pdf

  • Fan S, Zhao P, Yu C, Pan CP, Li X (2014) Simultaneous determination of 36 pesticide residues in spinach and cauliflower by LC–MS/MS using multi-walled carbon nanotubes-based dispersive solid-phase clean-up. Food Addit Contam (Part A) 31:73–82

    Article  CAS  Google Scholar 

  • Fantke P, Charles R, Alencastro LF, Friedrich R, Jolliet O (2011) Plant uptake of pesticides and human health, dynamic modeling of residues in wheat and ingestion intake. Chemosphere 85:1639–1647

    Article  CAS  PubMed  Google Scholar 

  • FAO/WHO Pesticide residues in food. (1989) Report of the joint meeting of the FAO panel of experts on pesticide residues in food and the environment and the WHO expert group on pesticide residues. FAO Plant Production and Protection 99

  • Ferrer C, Lozano A, Agüera A, Jiménez A, Fernández AR (2011) Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables. J Chromatogr A 1218:7634–7639

    Article  CAS  PubMed  Google Scholar 

  • Food and Agriculture Organization of the United Nations (FAO) (2014) FAO Statistical Databases available at http://faostat.fao.org (Accessed 21 June 2016)

  • Hajslova J, Zroslikova J (2003) Matrix effect in (ultra) trace analysis of pesticide residues in food and biotic matrices. J Chromatogr A 1000:181–197

    Article  CAS  PubMed  Google Scholar 

  • Hamilton D, Crossley S (2004) Pesticide residues in food and drinking water-human exposure and risks. Can J Cardiol 30(10):S354

    Google Scholar 

  • Han YT, Li WM, Dong FS, Xu J, Liu XG, Li Y, Kong ZQ, Liang XY, Zheng YQ (2013) The behavior of chlorpyrifos and its metabolite, 3,5,6-trichloro-2-pyridinol in tomatoes during home canning. Food Control 31(2):560–565

    Article  CAS  Google Scholar 

  • Han YT, Song L, Zhao PY, Li YJ, Zou N, Qin YH, Li X, Pan CP (2016) Residue determination of glufosinate in seedling origin foods using modified Quick Polar Pesticides (QuPPe) method and liquid chromatography coupled with tandem mass spectrometry. Food Chem 197(Part A):730–736

    Article  CAS  PubMed  Google Scholar 

  • He ZY, Wang L, Peng Y, Luo M, Wang WW, Liu XW (2015) Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method. Food Chem 169:372–380

    Article  CAS  PubMed  Google Scholar 

  • Hu JY, Hu YQ, Zhen ZH, Deng ZB (2011) Residue analysis of fluroxypyr-meptyl in wheat and soil by GC-ECD. Chromatographia 74:291–296

    Article  CAS  Google Scholar 

  • Johnson BD, Hall JC (1996) Fluroxypyr- and triclopyr-specific enzyme-linked immunosorbent assays, development and quantitation in soil and water. J Agric Food Chem 44(2):488–496

    Article  CAS  Google Scholar 

  • Kirkland KJ, Johnson EN, Stevenson FC (2001) Control of wild oat (Avena fatua) in wheat with MKH 6562. Weed Technol 15:48–55

    Article  CAS  Google Scholar 

  • Klinsunthorn N, Petsom A, Nhujak T (2011) Determination of steroids adulterated in liquid herbal medicines using QuEChERS sample preparation and high-performance liquid chromatography. J Pharmaceut Biomed 55(5):1175–1178

    Article  CAS  Google Scholar 

  • Lazartigues A, Thomas M, Cren-Olivé C, Brun-Bellut J, Le Roux Y, Banas D, Feidt C (2013) Pesticide pressure and fish farming in barrage pond in Northeastern France. Part II residues of 13 pesticides in water sediments edible fish and their relationships. Environ Sci Pollut Res 20:117–125

    Article  CAS  Google Scholar 

  • Lehmann RG, Miller JR (1989) Soil catalysed hydrolysis of fluroxypyr-methylheptyl ester. Weed Res 29(5):385–389

    Article  CAS  Google Scholar 

  • Lehotay SJ, Mastovská K, Lightfield AR (2005) Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. J AOAC Int 88:615–629

    CAS  PubMed  Google Scholar 

  • Malhat F, Watanabe H, Youssef A (2015) Degradation profile and safety evaluation of methomyl residues in tomato and soil. Hellenic Plant Protection Journal 8:55–62

    Article  Google Scholar 

  • Nguyen TD, Han EM, Seo MS, Kim SR, Yun MY, Lee DM, Lee GH (2008) 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

    Article  CAS  PubMed  Google Scholar 

  • Pang NN, Wang TL, Hu JY (2016) Method validation and dissipation kinetics of four herbicides in maize and soil using QuEChERS sample preparation and liquid chromatography tandem mass spectrometry. Food Chem 190:793–800

    Article  CAS  PubMed  Google Scholar 

  • Pareja L, Fernández-Alba AR, Cesio V, Heinzen H (2011) Analytical methods for pesticide residues in rice. Trends Anal Chem 30:270–297

    Article  CAS  Google Scholar 

  • Pastrana-Martínez LM, López-Ramón MV, Fontecha-Cámara MA, Moreno-Castilla C (2010) Batch and column adsorption of herbicide fluroxypyr on different types of activated carbons from water with varied degrees of hardness and alkalinity. Water Res 44:879–885

    Article  CAS  PubMed  Google Scholar 

  • Prado R, García R, Rioboo C, Herrero C, Abalde J, Cid A (2009) Comparison of the sensitivity of different toxicity test endpoints in a microalga exposed to the herbicide paraquat. Environ Int 35:240–247

    Article  CAS  PubMed  Google Scholar 

  • Ramesh A, Ravi PE (2001) Applications of solid-phase microextraction (SPME) in the determination of residues of certain herbicidesat trace levels in environmental samples. J Environ Monit 3:505–508

  • Tomlin CDS (2004) The e-pesticide manual, 13th edn. BCPC, Surry, p 380

    Google Scholar 

  • Walorczyk S (2014) Validation and use of a QuEChERS-based gas chromatographic-tandem mass spectrometric method for multiresidue pesticide analysis in blackcurrants including studies of matrix effects and estimation of measurement uncertainty. Talanta 120:106–113

    Article  CAS  PubMed  Google Scholar 

  • Wang L, Xu J, Zhao PY, Pan CP (2011) Dissipation and residues of fluroxypyr-meptyl in rice and environment. Bull Environ Contam Toxicol 86:449–453

    Article  CAS  PubMed  Google Scholar 

  • Yang YH, Kong WJ, Zhao LH, Xiao Q, Liu HM, Zhao XS, Yang MH (2015) A multiresidue method for simultaneous determination of 44 organophosphorous pesticides in Pogostemon cablin and related products using modified QuEChERS sample preparation procedure and GC–FPD. J Chromatogr B 974:118–125

    Article  CAS  Google Scholar 

  • Zhao HH, Xu J, DONG FS, Liu XG, Wu YB, Wu XH, Zheng YQ (2015) Simultaneous determination of three herbicides in wheat, wheat straw, and soil using a quick, easy, cheap, effective, rugged, and safe method with ultra high performance liquid chromatography and tandem mass spectrometry. J Sep Sci 38:1164–1171

    Article  CAS  PubMed  Google Scholar 

  • Zhao HY, Xue JY, Jiang NW, Peng W, Liu FM (2012) Dissipation and residue of fenpropidin in wheat and soil under field conditions. Ecotoxicol Environ Saf 77:52–56

    Article  CAS  PubMed  Google Scholar 

  • Zhao Q, Wei F, Luo YB, Ding J, Xiao N, Feng YQ (2011) Rapid magnetic solid-phase extraction based on magnetic multiwalled carbon nanotubes for the determination of polycyclic aromatic hydrocarbons in edible oils. J Agric Food Chem 59:12794–12800

    Article  CAS  PubMed  Google Scholar 

Download references

Funding

This study was partly funded by the Special Fund for Agroscientific Research in the Public Interest of China (grant number: 201503107).

Author information

Authors and Affiliations

  1. Department of Applied Chemistry, College of Science, China Agricultural University, Beijing, 100193, People’s Republic of China

    Fan Hou, Chong Chen, Fengmao Liu, Qingrong Peng & Peipei Teng

Authors
  1. Fan Hou
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Chong Chen
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Fengmao Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Qingrong Peng
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Peipei Teng
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Fengmao Liu.

Ethics declarations

Conflict of Interest

Fan Hou declares that she has no conflict of interest. Chong Chen declares that she has no conflict of interest. Fengmao Liu declares that he has no conflict of interest. Qingrong Peng declares that she has no conflict of interest. Peipei Teng declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Hou, F., Chen, C., Liu, F. et al. Trace Analysis of Fluroxypyr-Meptyl and Fluroxypyr in Wheat and Soil Ecosystem Based on Ion Column-Solid Phase Extraction Method and Liquid Chromatography-Tandem Mass Spectrometry. Food Anal. Methods 11, 2261–2271 (2018). https://doi.org/10.1007/s12161-018-1210-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-018-1210-5

Keywords

Search

Navigation