作　　者： ; ; ; ;

机构地区： 辽宁出入境检验检疫局

出　　处： 《中国粮油学报》 2003年第2期79-84,共6页

摘　　要： 本文研究了用高效液相色谱 -紫外检测器方法同时检测大米中八种氨基甲酸酯类农药 (杀线威、灭多威、涕灭威、抗芽威、残杀威、苯恶威、西维因、仲丁威 )的残留量。本文对多种氨基甲酸酯农药的提取、净化方法、色谱分离条件、线性关系、回收率和重现性进行了研究 ,并对方法进行了验证 ,研究结果表明用丙酮作为提取剂 ,用florisil和C18固相萃取净化柱双柱净化样品 ,简化了净化操作 ,且提高了检测灵敏度。采用SpherisorbC8色谱柱 ,流动相用乙腈 :水 (33.5∶6 6 .5 ) ,八种氨基甲酸酯类农药得到完全分离。八种氨基甲酸酯类农药的平均回收率分别为杀线威 80 .9%～ 89.5 % ,灭多威 82 .9%～ 91.6 % ,涕灭威 82 .6～ 91.2 % ,抗芽威 81.2 %～ 86 .7% ,残杀威 82 .3%～ 93.9% ,苯恶威 84 .7%～ 94 .4 % ,西维因82 .4 %～ 90 .0 % ,仲丁威 83.1%～ 91.0 %。变异系数 (Cv % )均在 3.97以下 ,检测低限分别为 :杀线威 0 .0 0 5 ,灭多威 0 .0 1,涕灭威 0 .0 0 5 ,抗芽威 0 .0 0 5 ,残杀威 0 .0 0 2 5 ,苯恶威 0 .0 0 2 5 ,西维因 0 .0 0 5 ,仲丁威 0 .0 1。方法的检测低限、回收率和精密度均满足残留分析要求。 In this paper,a liquid chromatographic method for the simultaneous determination of 8 carbamate pesticides in rice by UV detector is described.Eight carbamate pesticides include oxamyl, methomyl, aldicarb, pirimicarb, propoxur, bendiocarb, carbaryl and BPMC.The sample pretreatment method and the chromatographic parameters were optimized, and the recovery, repeatability and linear relationship were studied. The experiment result shows that eight carbamate pesticides can be separated on a spherisorb C_8 column, eluted with 33.5∶66.5(V/V)CH_3CN-H_2O as mobile phase. The pesticides were extracted with acetone and isolated from rice samples by using a double solid-phase extraction procedure with florisil and C_ 18 solid-phase columns. The average recoveries of 8 carbamates by using this method are as follows:oxamyl 80.9%-89.5%,methomyl 82.9%-91.6%,adicarb 82.6%-91.2%,pirimicarb 81.2%-86.7%,propoxur 82.3%-93.9%,bendiocarb 84.7%-94.4%,carbaryl 82.4%-90.0%,and fenobucarb 83.1%-91.0%. Repeatability coefficients of variation are less than 3.97%,and the detection limits are as follows:oxamyl 0.01mg/kg, methomyl 0.01mg/kg, adicarb 5g/kg, pirimicarb 0.01 mg/kg, propoxur 3g/kg, bendiocarb 3g/kg,carbaryl 5g/kg, fenobucarb 0.01mg/kg. The detection limits, recovery and repeatability indicate that the proposed method is well suitable for monitoring carbamate pesticides.

关 键 词： 双柱固相萃取 高效液相色谱法 测定 大米 氨基甲酸酯类农药残留量 净化 回收率 重现性

领　　域： [轻工技术与工程] [轻工技术与工程] [轻工技术与工程] [轻工技术与工程]