農產品中有機磷劑農藥美文松、二硫松及馬拉松殘留量檢驗方法之探討

ANALYTICAL METHODS FOR THE RESIDUES OF MEVINPHOS,DISULFOTON AND MALATHION IN CROPS

為配合衛生署77年4月公告農藥殘留容許量標準，本研究參照國內外文獻資料，進行有機磷劑農藥美文松、二硫松、馬拉松於農產品中殘留量檢驗方法之建立與探討。美文松利用丙酮萃取，經活性炭淨化，再以三氯甲烷抽取，以氣相層析儀附火焰光度檢出器測之；結果於特作類、根菜類添加2.5、5.0及7.5μg，回收率為83.0%～95.1%；於瓜菜類、包葉菜類、小葉菜類、果菜類添加12.5、25及37.5μg，回收率為84.2%～107.4%，最低檢出量為0.015ppm。二硫松利用乙腈萃取，再以二氯甲烷進行抽取，經氧化鋁淨化，以正己烷沖提後，以氣相層析儀附火焰光度檢出器測之；結果於米類、乾豆類、包葉菜類、小葉菜類及豆菜類添加2.5、5.0及7.5μg，回收率為84.2%～109.4%，於大漿果類添加12.5、25及37.5μg，回收率為97.0%～99.7%，最低檢出量為O.O1ppm、馬拉松利用乙腈萃取，再以二氯甲烷進行抽取，經Sep-Pak Silica Cartriedge淨化，以10%乙酸乙酯正己烷溶液沖提後，以氣相層析儀附火焰光度檢出器測之；結果於米類添加2.5 、5.0及7.5μg，回收率為101.9%～105.5%；於大漿果類及瓜菜類添加25、50及75μg，回收率為85.7～109.8%；於包葉菜類、小葉菜類、豆菜類及柑桔類添加50、100及150μg，回收率為84.2%～106.1%，最低檢出量為0.01ppm。本實驗經實際添加於各類作物所得回收率、再現性及最低偵測極限之結果良好得知，以上之三種檢驗方法均各別適用於美文松、二硫松及馬拉松其已公告容許量標準之各類作物。

Mevinphos residue was extracted from crops by homogenizing with acetone, cleaned up by charcoal, and partitioned with chloroform,then analyzed by GC-FPD (Gas Chromatography-Flame Photometric Detector).Six crops which had been set with tolerance were fortified with mevinphos standard solution at the level of 0.05-0.75 ppm. The average recoveries ranged from 83.0% to 107.4%. The detection limit of GC method for determination of mevinphos residue was 0.015 ppm. Disulfoton residue was extracted from crops by homogenizing with acetonitrile and partitioned with dichloromethane, then cleaned up by alumina column and analyzed by GC-FPD. Six crops which had been set with tolerance were fortified with disulfoton standard solution at the level of 0.05-0. 75ppm. The average recoveries ranged from 84.2% to 109.4%. The detection limit of GC method for disulfoton was 0.01ppm. Malathion residue was extracted from crops by homogenizing with acetonitrile and partitioned with dichloromethane, then cleaned up by silica cartridge, and analyzed by GC-FPD. Seven crops which had been set with tolerance were fortified with malathion standard solution at the level of 0.05-3.0ppm. The average recoveries ranged from 84.2% to 109.8%. The detection limit of GC method for determination of malathion residue was 0.01 ppm. Satisfactory recoveries and reproducibilities had been obtained in above three methods. Thus, these methods could be adopted as analytical methods in routine work.