Determination of Phorate (0,0-diethyl S-ethylthiomethyl phosphorithioate) and its Metabolites in Soil and Vegetables by GLC

토양(土壤)과 채소중(菜蔬中) Phorate(0,0-diethyl S-ethylthiomethyl phosphorithioate)와 그 대사산물(代謝産物)들의 GLC분석(分析)

Gas chromatographic method for the analysis of phorate(0,0-diethyl S-ethyl-thiomethyl phosphorithioate) and its metabolites in soil and vegetables was studied by using a mixed phase column(10% DC-200+8% Reoplex-400+2% QF-1 on Gas Chrom Q, $1.8{\times}2mm$ i.d, borosilicate glass column). This column can separate completely phorate and its four metabolites except phoratoxon sulfoxide. Retention time of standard mixture ranged 1.8 to 16.1 minutes at column temperature programming from 130 to $200^{\circ}C$ at $5^{\circ}C/min$ and detector sensitivity was also very high(0.05 to 1.05ng). Recoveries from soil and vegetables untreated but fortified with phorate and its three major metabolites at 0.05 and 0.5ppm levels were above 90% for phorate, phorate sulfoxide and phorate sulfone while recovery of phoratoxon metabolite was about 84%.

phorate와 그 대사산물(代謝産物)들의 잔류분(殘留分) 분석방법(分析方法)을 확립(確立)코자 10% DC-200+8% Reoplex-400+2% QF-1(2 : 1 : 1, w/w/w) on Gas Chrom Q( $80{\sim}100$ mesh), $1.8m{\times}2mm$ ID, borosilicate glass column인 mixed phase column을 이용(利用), flame photometric detector가 부착(附着)된 gas chromatograph로 조사(調査)하였다. 본(本) mixed phase column은 비록 phorate와 5가지 대사산물(代謝産物)을 동시(同時)에 분리(分離)하지는 못하였으나 column온도(溫度)를 programming$(130{\sim}200^{\circ}C,\;5^{\circ}C/min)$함으로써 phoratoxon sulfoxide를 제외(除外)한 5가지 화합물(化合物)의 분리(分離)가 가능(可能)하였다(phoratoxon sulfoxide는 phoratoxon과 중첩되었음). 또는 검출감도(檢出感度)도 매우 높아 $0.05{\sim}3.15ng$범위(範圍)이었다. 한편 토양(土壤)과 채소(菜蔬)에 처리(處理)한 phorate와 그 대사산물(代謝産物)들을 methanol-acetone-benzene(1 : 1 : 1, v/v/v)으로 Soxhlet장치(裝置)에서 12시간(12時間) 추출(抽出)한 후 benzene으로 이들 화합물(化合物)을 분리(分離)한 결과(結果) 90%이상(以上)의 높은 회수율(回收率)(phoratoxon은 약(約) 84%)을 얻었다. 따라서 본(本) mixed phase column은 분리(分離)와 감도면(感度面)에서 그 성능(性能)이 우수(優秀)하여 phorate의 분해(分解)와 대사(代謝)의 연구(硏究)에 효율적(效率的)으로 이용될 수 있을 것이다.