Article Detail

Home > Article Detail
  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

Development and validation of an analytical method for the determination of lepimectin residues by HPLC-PDA

Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2013, v.26 no.2, pp.142-153
https://doi.org/10.5806/AST.2013.26.2.142







  • Downloaded
  • Viewed

Abstract

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl (NH2) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient (R2)of both lepimectin A3 and A4 solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate,rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

keywords
lepimectin, HPLC-PDA, agricultural commodities, LOD, LOQ


Reference

1

 Alanwood, http://alanwood.net/pesticides/index

2

 KFDA. Korea Food Code. Korea Food and DrugAdministration, Seoul, Korea (2011).

3

 2012 작물보호제(농약) 지침서. 한국작물보호협회 (2012).

4

 M. H. Jeong, S. S. Hong, K. H. Park, J. E. Park, S. J. Kwack, Y. B. Kim, B. S. Han and W. C. Son, Korean Journal of Pesticide Science, 15(2), 218-229 (2011).

5

 KFDA, http://fse.foodnara.go.kr/residue/pesticides/ pesticides_info_view.jsp#ADI

6

 AOAC, Pesticide and industrial chemical residues, In official method of analysis, 17th ed, 1-88, AOAC International Arlington, VA, USA (2000).

7

 US FDA, Pesticide Analytical Manual, Vol 1: Multi residue Methods(3rd ed.) US Food and Drug Administration, USA (1999).

8

 식품공전 잔류농약 분석법 실무해설서, 이영득, KFDA (2012).

9

 Codex Alimentarius Commission, Guidelines on good laboratory practice in residue analysis, CAC/GL 40- 1993, Rome. Italy (2003).

10

 S. J. Lee, Y. H. Kim, L. W. Song, Y. S. Hwang, J. D. Lim, E. H. Sohn, M. H. Im, J. A. Do, J. H. Oh, K. S. Kwon, J. K. Lee, Y. D. Lee and M. G. Choung, Korean Journal of Pesticide Science, 15(3), 254-268 (2011).

11

 C. H. Kwon, M. H. Chang, M. H. Im, D. I. Choi, S. C. Jung, J. Y. Lee, Y. D. Yu, J. O. Lee and M. K. Hong, Anal. Sci. Technol., 21(6), 518-525 (2008).

상단으로 이동

Analytical Science and Technology