Browse > Article
http://dx.doi.org/10.7585/kjps.2013.17.4.264

Analysis of Systemic Pesticide Imidacloprid and Its Metabolites in Pepper using QuEChERS and LC-MS/MS  

Seo, Eun-Kyung (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Kim, Taek-Kyum (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Hong, Su-Myeong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Kwon, Hye-Yong (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Kwon, Ji-Hyung (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Son, Kyung-Ae (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Kim, Jang-Eok (School of Applied Biosciences, Kyungpook National University)
Kim, Doo-Ho (Department of Agro-food Safety, National Academy of Agriculture Science, Rural Development Administration)
Publication Information
The Korean Journal of Pesticide Science / v.17, no.4, 2013 , pp. 264-270 More about this Journal
Abstract
Imidacloprid is a systemic insecticide which act as an insect neurotoxin. It used for control of pest such as aphids and other sucking insects in fruits and vegetables. Systemic pesticides move inside a crop following absorption by the plant, and these were converted into a variety of metabolites. Sometimes these metabolites make a problem about safety of agricultural products. So a simultaneous determination method of pesticide and its metabolites is needed, to monitor their presence in agricultural product and study on the fate of pesticide in a plant. This study's aim is to investigate simultaneous analysis method of imidacloprid and its metabolites, imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, and 6-chloronicotinic acid in red pepper using QuEChERS method and LC-MS/MS systems. QuEChERS method was modifed beacuase $MgSO_4$ salts decreased the recoveries of 6-chloronicotinic acid in extraction procedure. Imidacloprid and its metabolites were extracted by acetonitrile with 1% glacial acetic acid and the extracts were purified through QuEChERS with primary secondary amine (PSA) and $C_{18}$ and analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.999. Recovery studies were carried out on spiked pepper blank sample at four concentration levels (0.01, 0.04 and 0.1, 0.4 mg/kg). The average recoveries of imidacloprid and its metabolites were in the range of 70~120% with < 20% RSD. This result indicated that the method using QuEChERS and LC-MS/MS was suitable for the simultaneous determination of imidacloprid and its metabolites in red pepper.
Keywords
QuEChERS; Systemic pesticide; Metabolites; Analysis method;
Citations & Related Records
Times Cited By KSCI : 2  (Citation Analysis)
연도 인용수 순위
1 Kamel, A. (2010) Refined methodology for the determination of neonicotinoid pesticides and their metabolites in Honey Bees and Bee products by liquid chromatography-tandem mass spectrometyr (LC-MS/MS). Journal of Agricultural and Food Chemistry. 58(10):5926-5931.   DOI   ScienceOn
2 Koesukwiwat, U., S. J. Lehotay, K. Mastovska, K. J. Dorweiler and N. Leepipatpiboon (2010) Extension of the QuEChERS Method for Pesticide Residues in Cereals to Flaxseeds, Peanuts, and Doughs. Journal of Agricultural and Food Chemistry. 58:5950-5958.   DOI   ScienceOn
3 Korea crop protection association (KCPA) 2012. pesticide application manual. seoul. Korea. p. 622-623.
4 Kwon, H. Y., C. S. Kim, B. J. Park, Y. D. Jin, K. A. Son, S. M. Hong, J. B. Lee and G. J. Im (2011) Multiresidue analysis of 240 pesticides in apple and lettuce by QuEChERS sample preparation and HPLC-MS/MS analysis. The Korean Journal of Pesticide Science. 15(4):417-433.   과학기술학회마을
5 Anastassiades, M., S. J. Lehotay, D. tajnbaher and F. J. Schenck (2003) Fast and Easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solidphase extraction” for the determination of pesticide residues in produce. Journal of AOAC International. 86:412-431.
6 Bong, M. S., S. Y. Yang, S. H. Lee, J. M. Seo and I. S. Kim (2011) Simultaneous analysis of conazole foungicides in garlic by Q-TOF mass spectrometer coupled with a modified QuEChERS method. Korean Journal of Environmnetal Agriculture. 30(3):323-329.   과학기술학회마을   DOI   ScienceOn
7 Lehotay, S. J. (2007) Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. Journal of AOAC International. 90(2):485-520.
8 Lehotay, S. J., K. A. Son, H. Y. Kwon, U. Koesukwiwat, W. Fu, K. Mastovska, E. Hoh and N. Leepipatpiboon (2010) Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. Journal of Chromatography A. 1217:2548-2560.   DOI   ScienceOn
9 Lesueur, C., P. Knittl, M. Gartner, A. Metntler and M. Fuerhacker (2008) Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuEChERS method. Food Control. 19:906-914.   DOI   ScienceOn
10 Nauen, R, K. Tietjen, K. Wanger and A. Elbert (1998) Efficacy of plant metabolites of imidacloprid against Myzus Persicae and (Homoptera : Aphididae), Pesticide Science. 52:53-57.   DOI
11 Nguyen, T. D., B. S. Lee, B. R. Lee, D. M. Lee and G. H. Lee (2007) 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 chromtography/mass spectrometry with temperature control and vaccum concentration. Rapid Communication in Mass Spectrometry. 22(18):3115-3122.
12 Nguyen, T. D., J. E. Yu, D. M. Lee and G. H. Lee (2008) A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry. Food Chemistry. 110:207-213.   DOI   ScienceOn
13 Paya, P., M. Anastassiades, D. Mark, I. Sigalova, B. Tasdelen, J. Oliva and A. Barba (2007) Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Analytical and Bioanalytical chemistry. 389(6):1697-1714.   DOI   ScienceOn
14 Tomizawa, M., H. Otsuka, T. Miyamoto, M. E. Eldefrawi and I. Yamamoto (1995) Pharmacological effects of imidacloprid and its realted compaounds on the nicotinic acetycholine receptor with its ion channel form the torpedo electric organ. Journal of Pesticide Science. 20:57-64.   DOI
15 Carretero, A. S., C. C. Blanco, S. P. Duran and A. F. Gutierrez (2003) Determination of imidacloprid and its metabolite 6-chloronicotinic acid in greenhouse air by application of micellar electrokinetic capillary chromatography with solidphase extraction. Journal of Chromatography A. 1003:189-195.   DOI   ScienceOn
16 HuSkova, R., E. Matisova, S. Hrouzkova and L. Svorc (2009) Analysis of pesticide residues by fast gas chromatography in combination with negative chemical ionization mass spectrometry. Journal of Chromatography A. 1216, 6326-6334.   DOI   ScienceOn
17 Schoning, R. and R. Schimuck (2003) Analytical determiation of imidacloprid and relevant metabolite residues by LC MS/ MS, Bulletin of Insectology, 56(1):41-50.
18 Suchail, S, D. Guez and L. P. Belzunces (2001) Discrepancy between acute and chronic toxicity induced by imidacloprid and its metabolites in Apis mellifera. Environmental Toxicology and Chemistry. 20(11):2482-2486.   DOI
19 Sur, R., and A. Stork (2003) Uptake, translocation and metabolism of imidacloprid in plant. Sulltetin of insectology, 56(1):35-40.
20 Xu, Y., L. F. Shou and Y. L. Wu (2011) Simultaneous determination of flonicamid and its metabolites in vegetables using QuEChERS and reverse-phase liquid chromatography-tandem mass spectrometry, Journal of Chromatography A. 1218:6663-6666.   DOI   ScienceOn