Determination of Buprofezin Residues in Rice and Fruits Using HPLC with LC/MS Confirmation
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초록
A high-performance liquid chromatographic (HPLC) method was developed to determine buprofezin residues in hulled rice and fruits. The buprofezin residue was extracted with acetone and the extract was stepwise purified by liquid-liquid partition and Florisil column chromatography. For rice samples, acetonitrile/n-hexane partition was additionally employed to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate buprofezin from sample co-extractives, as detected by ultraviolet absorption at 250 nm. Recovery experiment at the limit of quantitation validated that the proposed method could evidently determine the buprofezin residue at the level of 0.02 mg/kg. Mean recoveries from hulled rice, apple, pear, and persimmon samples fortified at three tenfold levels were in the range of 80.8~85.2%, 89.1~98.4%, 88.8~95.7% and 90.8~96.2%, respectively. Relative standard deviations of the analytical method were all less than 5%, irrespective of sample types. A selected-ion monitoring LC/mass spectrometry with positive electrospray ionization was also provided to sensitively confirm the suspected residue.
Abstract
A high-performance liquid chromatographic (HPLC) method was developed to determine buprofezin residues in hulled rice and fruits. The buprofezin residue was extracted with acetone and the extract was stepwise purified by liquid-liquid partition and Florisil column chromatography. For rice samples, acetonitrile/n-hexane partition was additionally employed to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate buprofezin from sample co-extractives, as detected by ultraviolet absorption at 250 nm. Recovery experiment at the limit of quantitation validated that the proposed method could evidently determine the buprofezin residue at the level of 0.02 mg/kg. Mean recoveries from hulled rice, apple, pear, and persimmon samples fortified at three tenfold levels were in the range of 80.8~85.2%, 89.1~98.4%, 88.8~95.7% and 90.8~96.2%, respectively. Relative standard deviations of the analytical method were all less than 5%, irrespective of sample types. A selected-ion monitoring LC/mass spectrometry with positive electrospray ionization was also provided to sensitively confirm the suspected residue.
참고문헌 (20)
- Ardrey, R. E., "Liquid chromatography-mass spectrometry:an introduction,pp.98-126,Wiley,Chichester,UK" (2003)
- Borges, J. H., "Analysis of pesticide residues in bananas harvested in the Canary islands (Spain)", Food Chemistry, 113, pp.313~319 (2009)
- Codex Alimentarius Commission(CAC), "Guidelines on good Laboratory practice in residue analysis", CAC, 2003, 1~2003
- Das, K. A., "Pesticide analysis", pp.425~453 (1981), Marcel Dekker
- Korea Crop Protection Association(KCPA), "Agrochemicals use guide book", pp.465~474 (2010), Agrochemicals use guide book
- Korea Food and Drug Administration(KFDA), "MRLs for pesticides in foods", 52~ (2009)
- Korea Food and Drug Administration(KFDA), "Analytical methods of pesticide residues in foods - In Korean code of food", ~ (2009)
- Lacina, O., "Identification", qunatification of multiple pesticide residues in food plants by ultra-high-performance liquid chromatography-time-of-flight mass spectrometry, 2010, pp.1217, 648~659
- Lee,Y. D., "High-performance liquid chromatographic determination of tricyclazole residues in rice grain", rice straw, and soil, Agric. Chem. Biotechnol., 41, pp.595~599 (1998)
- Lee,Y. D., "Multiresidue analysis of eight acaricides in fruits", Agric. Chem. Biotechnol, 42, pp.191~196 (1999)
- 이영득, "Determination of Monocrotophos Residues in Fruits and Soils Using High-Performance Liquid Chromatography", 한국환경농학회지, 23(4), pp.245~250 (2004), 한국환경농학회
- McLafferty, F. W., "Interpretation of mass spectra", pp.19~34, University Science Books, Sausalito
- Pesticide Residue Analysis Research Group(PRARG), "Analytical methods of pesticide residues", pp.128~130 (2006), Chuohoki Publishing
- Rural Development Administration(RDA), "Test guidelines for pesticide persistence. in: Criteria and Guidelines for Pesticide Registration" (2004)
- Santos, T. F. S., "Navickiene, S., 2008. MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography-mass spectrometry", Anal. Bioanal. Chem., 390, pp.1425~1430 (2008)
- Snyder, L. R., "Practical HPLC method development", pp.233~266 (1997), Wiley
- Soler, C., "Routine application using single quadrupole liquid chromatographymass spectrometry to pesticides analysis in citrus fruits", J. Chromatogr. A., 1088, pp.648~659 (2005)
- Tomlin, C. D. S., "The pesticide manual" (2009), British Crop protection Council
- US FDA, "Pesticide analytical manual, Vol 1: Multi-residue methods, 3rd ed." (1999), US Food and Drug Administration
- Zweig, G., "Analytical methods for pesticides and plant growth regulators Vol. XV, principles, statistics, and applications", pp.67~87 (1986), Academic Press