고단백질 함유 팥(Vigna angularis Willd.) 중 dithiocarbamate 살균제 mancozeb와 metiram 잔류분석법 개선 (Improvement of Analytical Method for Mancozeb and Metriram Residues in Red bean, Vigna angularis Willd with High Protein Content)

서지정보

· 발행기관 : 한국농약과학회
· 수록지 정보 : 농약과학회지 / 26권 / 3호 / 207 ~ 216페이지
· 저자명 : 함헌주, 임수빈, 허장현

초록

Dithiocarbamate계 살균제인 mancozeb와 metiram은 수용액과 유기용매에 난용성인 특징으로 잔류분석 시 추출 , 정제 방법이 매우 제한적인 화합물이다 . 최근 이 계열 농약의 잔류분석을 위하여 EDTA 수용액으로 추출한 후 methyl iodide로 유도체화하여 전처리하는 방법이 보편화되고 있다 . 그러나 이 분석법은 고함유 단백질을 포함하는 두류 시료의 경우 과량의 단백질에 의하여 methylation 유도체화 과정이 심하게 방해를 받아 분석 회수율이 매우 낮 은 문제점이 있다 . 본 연구는 고단백 함유 팥 시료에 대하여 단백질을 제거 과정을 적용한 후 dithiocarbamate계 살균 제인 mancozeb와 metiram에 대한 회수율 개선을 확인하고자 수행되었다 . 팥 시료에 대한 제단백 과정은 chlorform- gel method를 적용하였으며 , mancozeb의 회수율은 53.2 ± 10.0%(0회), 71.4 ± 4.7%(1회), 78.5 ± 9.0%(2회), 92.3 ± 2.4%(3회), 100.8 ± 3.3%(4회)이며 , metiram의 회수율은 51.3 ± 4.3%(0회), 71.7 ± 2.9%(1회), 80.4 ± 2.0%(2회), 92.3 ± 4.6%(3회), 101.5 ± 3.5%(4회)이었다 . 연구 결과 mancozeb와 metiram 잔류분석을 위한 팥 시료 중 제단백 과정은 3회가 적합한 것으로 판단하였다 . 제단백 과정을 적용한 개선된 잔류분석법은 정량한계 (LOQ) 0.01 mg kg-1, 회수율85.3~92.7%, 변동계수 2~10%로 유효성 검증기준을 충족하였다 . 본 분석법을 팥을 포함하는 두류 또는 단백질 함량 이 높은 농산물 등에 적용한다면 난분석 dithiocarbamate계 살균제의 잔류분석법 개선에 일조할 것으로 판단된다 .

영어초록

Mancozeb and metiram are a group of dithiocarbamate fungicides, poorly soluble in water and organic solvents, the methods used for extraction and purification during residue analysis are limited. Recently, a derivatization method in which extraction is performed using EDTA aqueous solution and methylated with methyl iodide for residue analysis of dithiocarbamates has become common. In addition, pulses samples, which are known with high protein content, could interfere with the methylation of dithiocarbamates and significantly reduce their recovery rates. Therefore, this study was conducted to improve the analytical method for mancozeb and metiram in red bean using HPLC/DAD and LC-MS/MS. To improve the accuracy of residue analysis, deproteinization was done followed by methylation. Deproteinization was performed multiple-times for each sample extract, and the recovery rates were observed. The recoveries obtained after deproteinization process were 53.2 ± 10.0% (no deproteinization), 71.4 ± 4.7% (1 time), 78.5 ± 9.0% (2 times), 92.3 ± 2.4% (3 times), and 100.8 ± 3.3% (4 times) for mancozeb. Whereas for metiram were 51.3 ± 4.3% (no deproteinization), 71.7 ± 2.9% (1 time), 80.4 ± 2.0% (2 times), 92.3 ± 4.6% (3 times), and 101.5 ± 3.5% (4 times). It was determined that the deproteinization process was suitable three times among red bean samples for residue analysis of mancozeb and metiram. The limit of quantitation (LOQ) for both compounds was 0.01 mg kg-1. The recovery yield of dithiocarbamates ranged from 85.3 to 92.7% with coefficient of variation 2.0~10.0%. Based on the finding, the current method could be applied to other dithiocarbamate groups in agricultural products containing high protein content and could contribute to the management system of pesticide safety.

참고자료

· 없음