Abstract
The dissipation and residues of an eco-friendly bio-pesticide, spinosad, in cowpea under field conditions were studied using ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MSMS) after Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction. The method exhibited good linearity with respect to spinosyn A and spinosyn D in solvent or blank cowpea matrix with correlation coefficients >0.99. Additionally, matrix effects were not significant in the range 0.987–1.014, and the average recoveries at three concentration levels were 75.1–91.1 and 79.4–90.5 % for spinosyn A and spinosyn D, respectively. The intra- and inter-day relative standard deviations were 2.5–9.3 and 7.8–9.8 % for spinosyn A, respectively, and 4.1–7.9 and 6.6–8.3 % for spinosyn D, respectively. The limits of detection (LODs) and limits of quantification (LOQs) were 0.005 and 0.01 mg kg−1, respectively, for spinosyn A, and 0.002 and 0.005 mg kg−1, respectively, for spinosyn D. The dissipation of spinosad (sum of spinosyn A and spinosyn D) fitted well to first-order kinetics with half-lives of 0.9–1.5 days. The highest residue (HR) at pre-harvest interval (PHI) of 12 h was 0.321 mg kg−1. Compared with the maximum residue limit (MRL) set by Codex, a PHI of at least 24 h was recommended. The estimated daily chronic intake of spinosad from cowpea was less than 0.14 % of the acceptable daily intake (ADI). Therefore, the risk of consuming cowpea sprayed with spinosad under recommended field conditions was considered acceptable for the Chinese population.
Similar content being viewed by others
References
Anastassiades, M., Lehotay, S. J., Stajnbaher, D., & Schenck, F. J. (2003). Fast and easy multiresidue method employing acetonitrile extraction/ partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. Journal of AOAC International, 86(2), 412–431.
Cleveland, C. B., Bormett, G. A., Saunders, D. G., Powers, F. L., McGibbon, A. S., Reeves, G. L., Rutherford, L., & Balcer, J. L. (2002). Environmental fate of spinosad. 1. Dissipation and degradation in aqueous systems. Journal of Agricultural and Food Chemistry, 50, 3244–3256.
Duan, Y., Guan, N., Li, P. P., Li, J. G., & Luo, J. H. (2016). Monitoring and dietary exposure assessment of pesticide residues in cowpea (Vigna unguiculata L. Walp) in Hainan, China. Food Control, 59, 250–255.
EFSA. (2012). Reasoned opinion on the review of the existing maximum residue levels (MRLs) for spinosad according to Article 12 of Regulation (EC) No 396/2005. EFSA Journal, 10(3), 2630.
EPA. (2000). Guidance for refining anticipated residue estimates for use in acute dietary probabilistic risk assessment. Washington.
EPA. (2013). Food safety. http://www.epa.gov/agriculture/tfsy.html. Accessed 14 Mar 2013
Hamilton, D., Ambrus, A., Dieterle, R., Felsot, A., Harris, C., Petersen, B., Racke, K., Wong, S. S., Gonzalez, R., Tanaka, K., Earl, M., Roberts, G., & Bhula, R. (2004). Pesticide resicues in food-acute dietary exposure. Pest Management Science, 60, 311–339.
Li, W. M., Qiao, C. K., Chen, X. X., Li, Q. Y., Li, M. H., Li, W. X., & Han, L. J. (2012). Study on decline and residue of spinosad in paddy using high performance liquid chromatography-tandem mass spectrometry. Chinese Journal of Pesticide Science, 14(3), 298–304.
Mai, C. Q., Wang, S., & Yuan, W. F. (2012). Preliminary study of green control technology and prediction method for cowpea thrips on cucurbits and vegetables in Sanya City, China. Plant Protection, 32(11), 43–45.
Malhat, F., Badawy, H. M. A., Barakat, D. A., & Saber, A. N. (2014). Residues, dissipation and safety evaluation of chromafenozide in strawberry under open field conditions. Food Chemistry, 152, 18–22.
Mandal, K., Jyot, G., & Singh, B. (2009). Dissipation kinetics of spinosad on Cauliflower (Brassica oleracea var. botrytis. L.) under subtropical conditions of Punjab, India. Bulletin of Environmental Contamination and Toxicology, 83, 808–811.
People’s Daily Online. (2010). Hainan toxic cowpeas concern spread; more provinces ban sale after tests reveal toxic pesticide contamination. http://en.people.cn/90001/90776/90882/6904282.html. Accessed 28 Feb 2010.
Pesticide Safety Directorate. (1998). Pesticide residues variability and acute dietary risk assessment. York.
SANCO/12571/2013. (2013). Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. http://www.eurl-pesticides.eu/library/docs/allcrl/AqcGuidance_Sanco_2013_12571.pdf. Accessed 2013
Sharma, A., Srivastava, A., Ram, B., & Srivastava, P. C. (2007). Dissipation behavior of spinosad insecticide in chilli and soil. Asian Journal of Water, Environment and Pollution, 5(2), 49–52.
Singh, S., & Battu, R. S. (2012). Dissipation kinetics of spinosad in cabbage (Brassica oleracea L.var.capitata). Toxicological & Environmental Chemistry, 94(2), 319–326.
Sun, M., Cao, Z. Y., Liu, H., Ma, Y. N., & Chen, M. X. (2010). Determination of spinosad in vegetables by PSA dispersive solid phase extraction and high performance liquid chromatography-mass spectrometry. Chinese Journal of Analysis Laboratory, 29(8), 70–74.
Watson, G. B. (2001). Actions of insecticidal spinosyns on g-amino-butyric acid responses from small-diameter cockroach neurons. Pesticide Biochemistry and Physiology, 71, 20–28.
West, S. D. (1996). Determination of the naturally derived insect control agent spinosad in cottonseed and processed commodities by high-performance liquid chromatography with ultraviolet detection. Journal of Agricultural and Food Chemistry, 44, 3170–3177.
West, S. D. (1997). Determination of the naturally derived insect control agent spinosad and its metabolites in soil, sediment, and water by high-performance liquid chromatography with ultraviolet detection. Journal of Agricultural and Food Chemistry, 45, 3107–3113.
West, S. D., Yeh, L. T., Turner, L. G., Schwedler, D. A., Thomas, A. D., & Duebelbeis, D. O. (2000). Determination of spinosad and its metabolites in food and environmental matrices. 1. High-performance liquid chromatography with ultraviolet detection. Journal of Agricultural and Food Chemistry, 48, 5131–5137.
WHO. (1997). Guidelines for predicting dietary intake of pesticide residues. 2nd revised edition, GEMS/Food Document WHO/FSF/FOS/97.7, Geneva.
WHO. (2009). Principles and methods for the risk assessment of chemicals in food. Environmental Health Criteria, 240.
Wu, R. F., Du, F. Z., & Luo, H. L. (2011). Identification and control of cowpea fusarium wilt. Journal of Changjiang Vegetables, 15, 45–46.
Xiao, C. L., Liu, Y., Wu, Q. J., Zhang, Y. J., Wu, Q. X., Yuan, T. Q., Luo, F., Wan, S. L., & Kong, X. Y. (2014). Toxicity of different pesticides to cowpea thrips Megalurothrips usitatus (Bagnall) in Sanya area. Plant Protection, 40(6), 164–166.
Yeh, L. T., Schwedler, D. A., Schelle, G. B., & Balcer, J. L. (1997). Application of Empore disk extraction for trace analysis of spinosad and metabolites in leafy vegetables, peppers, and tomatoes by high-performance liquid chromatography with ultraviolet detection. Journal of Agricultural and Food Chemistry, 45, 1746–1751.
Zhang, J., Yang, L. Z., Lin, L. Y., Chen, L. P., Zhou, Y., & Xu, D. M. (2011). Determination of spinosyns A and D residues in food by high performance liquid chromatography-tandem mass spectrometry. Chinese Journal of Chromatography, 29(7), 637–642.
Zhao, E. C., Xu, Y. J., Dong, M. F., Jiang, S. R., Zhou, Z. Q., & Han, L. J. (2007). Dissipation and residues of spinosad in eggplant and soil. Bulletin of Environmental Contamination and Toxicology, 78, 222–225.
Acknowledgments
This research was supported by the National Key Technology R&D Program of the Ministry of Science and Technology of China (No. 2012BAK01B00).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Huan, Z., Luo, J., Xu, Z. et al. Residues, dissipation, and risk assessment of spinosad in cowpea under open field conditions. Environ Monit Assess 187, 706 (2015). https://doi.org/10.1007/s10661-015-4942-3
Received:
Accepted:
Published:
DOI: https://doi.org/10.1007/s10661-015-4942-3