Krause R T, August E M
J Assoc Off Anal Chem. 1983 Mar;66(2):234-40.
Several fruits and vegetables were fortified at a low (0.02-0.5 ppm) and at a high (0.1-5 ppm) level with pesticides and with a synergist, and recoveries were determined. Analyses were performed by using 3 steps of a multiresidue method for determining N-methylcarbamates in crops: methanol extraction followed by removal of plant co-extractives by solvent partitioning and chromatography with a charcoal-silanized Celite column. Eleven compounds were determined by using a high performance liquid chromatograph equipped with a reverse phase column and a fluorescence detector. Twelve additional compounds were determined by using a gas-liquid chromatograph equipped with a nonpolar packed column and an electron capture or flame photometric detector. Recoveries of 10 pesticides (azinphos ethyl, azinphos methyl, azinphos methyl oxygen analog, carbaryl, carbofuran, naphthalene acetamide, naphthalene acetic acid methyl ester, napropamide, phosalone, and phosalone oxygen analog) and the synergist piperonyl butoxide, which were determined by high performance liquid chromatography, averaged 100% (range 86-117) at the low fortification level and 102% (range 93-115) at the high fortification level. Quantitative recovery of naphthalene acetamide through the method required that an additional portion of eluting solution be passed through the charcoal column. Recoveries of 7 additional pesticides (dimethoate, malathion, methyl parathion, mevinphos, parathion, phorate oxygen analog, and pronamide), which were determined by gas-liquid chromatography (GLC), averaged 108% (range 100-120) at the low fortification level and 107% (range 99-122) at the high fortification level. DDT, diazinon, dieldrin, phorate, and pirimiphos ethyl, which were determined by GLC, were not quantitatively recovered.
几种水果和蔬菜分别用低浓度（0.02 - 0.5 ppm）和高浓度（0.1 - 5 ppm）的农药及一种增效剂进行强化处理，并测定回收率。采用多残留方法的三个步骤对农作物中的N - 甲基氨基甲酸酯进行分析：先用甲醇提取，然后通过溶剂分配和用炭化硅烷化硅藻土柱进行色谱分离去除植物共提取物。使用配备反相柱和荧光检测器的高效液相色谱仪测定了11种化合物。另外12种化合物则使用配备非极性填充柱和电子捕获或火焰光度检测器的气液色谱仪进行测定。通过高效液相色谱法测定的10种农药（乙基谷硫磷、甲基谷硫磷、甲基谷硫磷氧类似物、西维因、克百威、萘乙酰胺、萘乙酸甲酯、敌草胺、伏杀硫磷和伏杀硫磷氧类似物）和增效剂胡椒基丁醚，在低强化水平下回收率平均为100%（范围86 - 117），在高强化水平下为102%（范围93 - 115）。通过该方法对萘乙酰胺进行定量回收需要额外一部分洗脱液通过炭柱。通过气液色谱法（GLC）测定的另外7种农药（乐果、马拉硫磷、甲基对硫磷、速灭磷、对硫磷、氧乐果和拿草特），在低强化水平下回收率平均为108%（范围100 - 120），在高强化水平下为107%（范围99 - 122）。通过气液色谱法测定的滴滴涕、二嗪农、狄氏剂、甲拌磷和乙基嘧啶磷未实现定量回收。
