Abstract |
Ion trap 질량분석기와 Quadrupole 질량분석기를 이용한 밀가루 중 유기인제(dimethoate, diazinon, parathion-methyl, fenitrothion, malathion) 및 인삼 중 BHC 이성질체들의 정성 정량 분석에 대한 유용성을 평가하기 위해 검출한계를 구하고, 검량선을 작성하였다. 이온화 방법으로 EI와 CI를 사용하여 mass fragmentation pattern을 비교하여 정성분석에 적용하였으며, scan과 selected ion monitoring(SIM) mode로 미량분석법으로서의 유용성을 평가하였다. 검출한계는 ion trap에서 scan시 0.008~0.225ng이었으며, quadrupole에서는 scan시 0.23~3.1ng, SIM 측정시 0.032~0.68ng으로 ion trap이 quadrupole의 scan시 보다 2~300배, SIM 보다 4~30배까지 검출한계가 낮았다. 검량선의 직선성은 ion trap과 quadrupole 모두 0.9 이상이었다. 밀가루 추출물은 Bio-Bead S-X3를 사용하여 정제하였고, 인삼은 Florisil column으로 정제하였다. 5종의 유기인제의 회수율은 80% 이상이었으며, BHCs의 회수율은 60~90%이었다. Detection limit as well as calibration curves on organophosphorus pesticide(dimethoate, diazinon, parathion-methyl, fenitrothion, malathion) and BHCs were measured for evaluation of utility on qualitative or quantitative analysis of pesticides with ion Trap mass spectrometer and quadrupole mass spectrometer. As ionization source, EI and CI were adopted for qualitative analysis of pesticides by comparison of each fragmentation pattern. At the same time, the utility as trace analysis techniques through scan or selected ion monitoring(SIM) mode was evaluated. With ion trap for all pesticides, detection limit(DL, 1 μL injection) on scan mode was ranged 0.008∼0.225 ng at signal to noise ratio 3. With quadrupole DL on scan mode was ranged 0.23∼3.1 ng over 0.032∼0.68 ng on SIM mode. The calibration curve with ion trap generated good linearity over 0.99 as correlation coefficient. As clean up procedure, Bio Beads S-X3 was used for the separation of oils from five organophosphorous pesticides in flour extractant showing more than 80% as recovery at most cases. In case of BHCs in jinseng with Florisil column, the recovery of pesticides has been 60% to 90%. |
