한약재 중 살충제 Endosulfan의 잔류분석을 위한Macroporous Diatomaceous Earth 컬럼 적용
Application of Macroporous Diatomaceous Earth Column for Residue Analysis of Insecticide Endosulfan in Herbal Medicines
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초록
현재 식품의약품안전청에서 고시하고 있는 한약재 중 잔류농약 분석법에 따라 강활, 박하, 천궁 및 황기 시료 중 endosulfan과그 분해산물인 endosulfan sulfate를 분석한 결과많은 간섭물질의 등장과 낮은 회수율 등의 문제점을 확인하였다. 이에 고시된 시험법의 액-액 분배 과정을 대신하여 MDE column을 적용하여 α-endosulfan 80.3 ~ 93.5%, β-endosulfan 81.0 ~ 100.3%, endosulfan sulfate 80.6 ~ 95.6%의회수율과 1.1 ~ 3.4%의 변이계수(CV)를 얻었으며 이러한 결과는 잔류농약 분석기준을 만족하였다. MDE column의 사용으로 액-액 분배 과정을 대신하면서 발암가능 물질인 dichloromethane 사용을 배제할 수 있어 분석자의 안전성 향상,노동력 및 전처리 시간의 절감, 발생되는 폐액 감소, 액-액 분배시 emulsion 현상의 해소, 분석자간의 재현성 양호 등의이점도 얻을 수 있었다.
Abstract
BACKGROUND: Because dried herbal medicines have many active ingredients, it is not easy to determine the residue amount after extraction, partition and clean up of pesticides from them. Especially, liquid-liquid partition method is consuming many times and solvents. Macroporous diatomaceous earth(MDE) column was used to replace the separatory funnel for liquid-liquid extraction with dichloromethane to analyze the endosulfan and its metabolite. METHODS AND RESULTS: The residue analysis method using MDE column instead of liquid-liquid partition for determining insecticide endosulfan and its metabolite in 4 dried herbal medicines was developed by GC/MS. As a result, the recovery rates of the pesticides in 4 herbal medicines were ranged from 80.3 to 93.5% for α-endosulfan, from 81.0 to 100.3% for β-endosulfan and from 80.6 to 95.6% for endosulfan sulfate, respectively. The coefficients of variation for triplicate were ranged from 1.1 to 3.4%. CONCLUSION: The improved methods are more eco-friendly, safer, faster and less laborious than conventional method by KFDA.
참고문헌 (18)
- Iijima, K., "Multiresidue analytical method of pesticides by GC-MS : application of macroporous diatomaceous earth column and silica gel cartridge", J. Pest. Sci, 22, pp.17~26 (1997)
- Iijima, K., "Application of combination column of macroporous diatomaceous earth and graphitized carbon black for pesticide residue analysis", J. Pest. Sci, 22, pp.17~26 (2006)
- International Agency for Research on Cancer, "Overall evaluations of carcinogenicity : An updating of IARC Monographs volume 1 to 42", United Kingdom, 194~195 (1987)
- Klein, J, "Applicability of gradient liquid chromatography with tandem mass spectrometry to the simultaneous screening for about 100 pesticides in crops", J. AOAC Int., 86, pp.1015~1037 (2003)
- Kobayashi, M, "Clean-up method of forchlorfenuron in agricultural produts for HPLC analysis", J. Food Hyg. Soc. Japan, 48(5), pp.148~152 (2007)
- Korea Crop Protection Association, "Pesticides Use Guidelines for 2010", pp.47~1131 (2010), Samjeung press
- Korea Food and Drug Administration, "Information for Production Region of Herbal Medicines in China", 1~ (2009)
- Korean Society of Food and Technology, "Encyclopedia of Food Science and Technology", pp.131~ (2004), Kwangil
- 이주희, "한약재 진피에 대한 유기인계 살충제의 잠정 MRL 설정 및 안전사용기준 제안", 한국환경농학회지, 29(1), pp.66~71 (2010), 한국환경농학회
- Oh, C.H, "Monitoring of Residual Pesticides in Herbal Drug Materials of Korea and China", BULLETIN OF ENVIRONMENTAL CONTAMINATION AND TOXICOLOGY, 82(0), pp.639~643 (2009), Springer
- Qian, G., "A multiresidue method for 20 pesticides in Radix paeoniae alba of Chinese herbal by gas chromatography with electron-capture detection", Bull Environ. Contam. Toxicol, 84, pp.779~783 (2010)
- Stajnbaher, D, "Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatography-mass spectrometry", J. Chromatogr. A, 1015, pp.185~198 (2003)
- Sicbaldi, F., "Diatomaceous earth-assisted extraction for multiresidue determination of pesticides", J. Chromatogr. A, 765, pp.23~30 (1997)
- Tseng, S.H., "Determination of butachlor and pencycuron residues in vegetables and rice: application of the macroporous diatomaceous earth column", J. Food Drug Anal, 10, pp.127~134 (2002)
- Tseng, S.H., "A multiresidue method for determining 136 pesticides and metabolites in fruits and vegetable : Application of macroporous diatomaceous earth column", J. Food Drug Anal, 15(3), pp.316~324 (2007)
- Watanabe, E, "Simultaneous Determination of Neonicotinoid Insecticides in Agricultural Samples by Solid-Phase Extraction Cleanup and Liquid Chromatography Equipped with Diode-Array Detection", J. Agric. Food Chem, 55, pp.3798~9804 (2007)
- Wong, J.W., "Multiresidue pesticide analysis of ginseng powders using acetonitrile-or acetone-based extraction,solid-phase extraction cleanup,and gas chromatography-mass spectrometry", selective ion monitoring(GC-MS, MS),J.Agric.Food Chem.58,5884-5896, pp.J. Agric. Food Chem, 2010[DOI]
- Wu, J., "Dynamic of carbendazim residue in panax notoginseng and soil", Bull Environ. Contam. Toxicol, 84, pp.469~472 (2010)