Abstract
A method for the simultaneous analysis of 31 residual organic chloride pesticides was studied using gas chromatography. Prepared analytical samples were injected to gas chromatography (HP 5890 Series II plus) on the Ultra-2 column with ECD. The packing materials for column were changed as the following reagents ; florisil and alumina N, The residual solution was loaded to column and was elected pith erection solvents ; ether : benzene (2 : 8) solution, hexane : benzene (1 : 1) solution, dichloromethane, acetone, and methanol. The analytical results showed that 6 kinds of organic chlorides were not detected when florisil (first condition) was used as the column packing material. The nondetected 6 kinds of organic chlorides in the first analytical condition were detected and the recoveries of thrin-pesticides were increased, in particular, captan and captafol, but the recoveries of benzene hexachloride compounds were decreased when dichloromethane and methanol were added as elution solvents (pac'king material was florisil as in the first condition). The recoveries of dichlornuanid, chlorofenvinfos, folpet, and dicofol were increased and that of aldrin was increased, but those of captan and captafol were not good when alumina N was used as the packing material. To detect simultaneously thrin-pesticides, captan, and captafol, florisil and alumina N were used as the packing materials. The elution result showed that captan and captafol were not detected. This was because the column was activated insufficiently. The analytical method was the best (31 kinds of organic chlorides in the residual pesticides were detected sharply and showed high sensitivity) when the column (packing materials were florisil and alumina N: together) was fuliy activated and the impurities were removed using various elution solvents.
31 종류의 유기 염소계 잔류 농약을 동시에 분석하는 기체 크로마토그래피 방법을 개발하기 위하여 본 연구를 수행하였다. 준비된 분석 시료를 ECD (electron capture detector)로 Ultra-2 column의 GC (gas chromatography)에 주입하였다. Column 충진 물질을 florisil과 alumina N으로 변화시키면서 잔류 용액을 column에 loading하고 용출 용매로는 ether . benzene(2 : 8) solution, hexane . benzene(1 . 1) solution, dichloromethane, acetone 및 methanol을 사용하였다. 분석 결과 column 충진 물질로 florisil을 사용하였을때 (첫째 조건) 6종류의 유기 염소(dichlorfluanid, captan, chlorofenvinfos, folpet, captafol과 dicofol)가 검출되지 않았다. 이 조건에서 dichloromethane과 methanol을 용출 용매로 첨가하였을때는 (둘째 조건) 첫째 분석 조건하에서 검출되지 않았던 6종류의 유기 염소가 검출되었고 thrin계 pesticides, 특히 captan과 captafol의 recovery가 증가하였다(첫째 조건에서와 마찬가지로 충진 물질로 florisil을 사용). 그러나 BHC(benzene hexachloride) 화합물의 recovery는 감 소하였다. 한편 alumina N을 column 충진 물질로 사용하였을 경우에는 dichlorfluanid, chlorofenvinfos, folpet 및 dicofol의 recovery가 증가하였으며 aldrin도 그러하였다. 하지만 captan과 captafol은 그렇지 못하였다. Thrin계 pesticides, captan 및 captafol을 동시에 검출하기 위하여 florisil과 alumina N을 충진 물질로 동시에 사용하고 n-hexane을 충진시켜 용출시킨 결과, captan과 captafol이 검출되지 않았는데 이는 column이 충분히 활성화되지 않았기 때문이라고 생각된다. Column(florisil과 alumina N을 충진 물질로 동시 사용)을 충분히 활성화시키고 여러가지 용출 용매를 사용하여 불순물을 제거하였을때 분석 결과가 가장 우수하였다(31 종류의 유기 염소계 잔류 농약이 sharp하게 검출되었고 높은 감도를 나타내었다).