Abstract
In this study, an optimized QuEChERS method with liquid chromatography-tandem mass spectrometry (LC–MS/MS) was developed and validated for the determination of mesosulfuron-methyl and diflufenican in wheat grain and straw. At the spiking levels of 0.01, 0.02, 0.05, 0.1, and 1 mg/kg, the average recoveries of five repetitions were 74–98% with RSDs of 1–11%. The LOQs of the two herbicides were both 0.01 mg/kg for wheat grain and wheat straw. The ultimate residues of field trials in ten regions were mostly lower than LOQ (0.01 mg/kg), except that the residue of mesosulfuron-methyl in wheat straw in Hubei Province was 0.015 mg/kg and the residue of diflufenican in wheat straw in Shaanxi Province was 0.028 mg/kg. Long-term dietary risk assessment indicated that hazard quotients were 0.0014% and 0.031% for mesosulfuron-methyl and diflufenican, respectively, which means that it is safe to spray the two herbicides on wheat at the recommended dosage.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
Data Availability
The authors declare that all other data supporting the findings of this study are available within the article and its supplementary information files.
References
Akiyama Y, Matsuoka T, Mitsuhashi T (2009) Multi-residue screening method of acidic pesticides in agricultural products by liquid chromatography/time of flight mass spectrometry. J Pestic Sci 34(4):265–272. https://doi.org/10.1584/jpestics.G09-29
Angel Gonzalez-Curbelo M, Lehotay SJ, Hernandez-Borges J, Angel Rodriguez-Delgado M (2014) Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast, low-pressure gas chromatography and liquid chromatography tandem mass spectrometry. J Chromatogr A 1358:75–84. https://doi.org/10.1016/j.chroma.2014.06.104
Bi YY, Han LJ, Song SY, Yao W, Qin FY, Xu YJ, Wu Q (2020) Method validation, storage stability and field trial for residues of florasulam and pyroxsulam in cereal by liquid chromatography with tandem mass spectrometry. Food Addit Contam, Part A 37(5):793–803. https://doi.org/10.1080/19440049.2020.1723809
Conte E, Morali G, Galli M, Imbroglini G, Leake CR (1998) Long-term degradation and potential plant uptake of diflufenican under field conditions. J Agric Food Chem 46(11):4766–4770. https://doi.org/10.1021/jf980190l
[EFSA] European Food Safety Authority (2007) Conclusion regarding the peer review of the pesticide risk assessment of the active substance-diflufenican. EFSA Scientific Report 122:1–84
[EFSA] European Food Safety Authority (2016) Peer review of the pesticide risk assessment of the active substance mesosulfuron (variant evaluated mesosulfuron-methyl). EFSA J 14(10):4584
[FAO/WHO] Food and Agriculture Organization of the United Nations/ World Health Organization (1988) Guidelines for predicting the dietary-intake of pesticide-residues. Bull w h o 66(4):429–434
Haynes C, Kirkwood RC (1992) Studies on the mode of action of diflufenican in selected crop and weed species-basis of selectivity of preemergence and early postemergence applications. Pestic Sci 35(2):161–165. https://doi.org/10.1002/ps.2780350210
Lehotay SJ, Mastovska K, Yun SJ (2005) Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes. J AOAC Int 88(2):630–638
Li MM, Liu XG, Dong FS, Xu J, Kong ZQ, Li YB, Zheng YQ (2013) Simultaneous determination of cyflumetofen and its main metabolite residues in samples of plant and animal origin using multi-walled carbon nanotubes in dispersive solid-phase extraction and ultrahigh performance liquid chromatography-tandem mass spectrometry. J Chromatogr A 1300:95–103. https://doi.org/10.1016/j.chroma.2013.05.052
Liu L, Shao H, Li H, Li N, Li J, Song SR, Zhang YT, Guo YZ (2015) Determination of diflufenican residues in wheat by UPLC- MS/MS. Agrochemicals 54(6):431–433
Lorenz K, Willms L, Muller KH (2005) Mesosulfuron-methyl, a new grass herbicide for cereal production. Pflan Nach Bayer 58(2):171–178
Lu Z, Hou ZG (2020) Dissipation and residues of diflufenican in rice. J Jilin Agric Univ 42(5):576–580. https://doi.org/10.13327/j.jjluu.2020.6055
Mastovska K, Dorweiler KJ, Lehotay SJ, Wegscheid JS, Szpylka KA (2010) Pesticide multiresidue analysis in cereal grains using modified QuEChERS method combined with automated direct sample introduction GC-TOFMS and UPLC-MS/MS techniques. J Agric Food Chem 58(10):5959–5972. https://doi.org/10.1021/jf9029892
Matuszewski BK, Constanzer ML, Chavez-Eng CM (2003) Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS. Anal Chem 75(13):3019–3030. https://doi.org/10.1021/ac020361s
Ni YX, Yang H, Zhang HT, He QA, Huang SQ, Qin ML, Chai SS, Gao HH, Ma YN (2018) Analysis of four sulfonylurea herbicides in cereals using modified Quick, Easy, Cheap, Effective, Rugged, and Safe sample preparation method coupled with liquid chromatography-tandem mass spectrometry. J Chromatogr A 1537:27–34. https://doi.org/10.1016/j.chroma.2018.01.017
Saxena R, Tomar RS, Kumar M (2016) Allelopathy: a green approach for weed management and crop production. Int J Curr Res Biosci Plant Biol 3(4):43–50. https://doi.org/10.20546/ijcrbp.2016.304.008
WHO World Health Organization (1997) Guidelines for predicting dietary intake of pesticide residues/prepared by the Global Environment Monitoring System – Food Contamination Monitoring and Assessment Programme (GEMS/Food); in collaboration with the Codex Committee on Pesticide Residues. Rev. ed. Geneva (Switzerland): Programme of Food Safety and Food Aid, World Health Organization. Global Environment Monitoring System. Food Contamination and Monitoring Programme & Joint FAO/WHO Codex Alimentarius Commission. Committee on Pesticide Residues.
Yao W, Zhang ZH, Song SY, Hao XH, Xu YJ, Han LJ (2019) Multi-residue analysis of 34 pesticides in black pepper by QuEChERS with d-SPE Vs. d-SLE cleanup. Food Anal Methods 12(1):176–189. https://doi.org/10.1007/s12161-018-1350-7
Zhang SJ, Yang GL, Zheng ZS, Chen YD, Wang L, Qian X (2009) Study on the residue dynamics of mesosulfuron-methyl in wheat and soil. J Hebei Agric Univ 32(3):12–16
Funding
The current study was funded by the National Key R&D Program of China, grant number 2017YFD800700.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Ethics Approval
This article does not contain any studies with human participants or animals performed by any of the authors.
Consent to Participate
Informed consent was obtained from all individual participants included in the study.
Conflict of Interest
Fayi Qin declares that he has no conflict of interest. Yingying Bi declares that she has no conflict of interest. Lijun Han declares that she has no conflict of interest. Shuangyu Song declares that she has no conflict of interest. Xinru Lv declares that she has no conflict of interest.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Supplementary Information
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Qin, F., Bi, Y., Han, L. et al. Method Validation and Residue Analysis of Mesosulfuron-Methyl and Diflufenican in Wheat Field Trial by Liquid Chromatography with Tandem Mass Spectrometry. Food Anal. Methods 15, 2617–2624 (2022). https://doi.org/10.1007/s12161-022-02296-1
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-022-02296-1