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Method Validation for the Estimation of Organochlorine Insecticides in Potato

机译:马铃薯中有机氯杀虫剂估算方法的验证

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The study was undertaken to validate the method of analysis for nine organochlorine insecticides namely α-HCH, γ-HCH, heptachlorexoepoxide, heptachlorendoepoxide, aldrin, dieldrin, 2,4 DDT, β-endosulfan, endosulfansulphate in potato. The insecticides were extracted in acetone, partitioned into DCM:Hexane (1:1, v/v), cleaned up by adsorption chromatography on glass column (60 cm x 2 cm id) with purified silica gel (60-120 mesh) and eluted with 200 ml of mixture of dichloromethane: acetone (1:1, v/v). The pesticides were estimated by GC equipped with ~(63)Ni electron capture detector (ECD) and BP, column (30 m x 0.025 mm id) packed with 100% dimethylpolysiloxane. The accuracy, precision and method LOQ (limit of quantification) determined via recovery experiments at their respective spiking levels ranged from 0.0018-0.0072 ug/g with the recoveries of ≥ 85%. The limit of detection (LOD) varied from 0.0005-0.0012. The standard deviation ranged from 0.0006 - 0.0018 while the % RSD ranged from 2.74-13.47. Good linearity (at least r~2≥0.99) of the calibration curve was obtained over the range of 0.001 -0.45 μg/ml. The data for detection limits, mean % recovery and % relative standard deviation revealed that method is acceptable for estimation of all the nine insecticides studied in potato.
机译:进行该研究以验证分析马铃薯中9种有机氯杀虫剂的方法,即α-HCH,γ-HCH,七氯环己氧化物,七氯内环氧化物,艾氏剂,狄氏剂,2,4滴滴涕,β-硫丹,硫丹硫酸盐。将杀虫剂在丙酮中萃取,分配到DCM:己烷(1:1,v / v)中,在玻璃柱(60 cm x 2 cm内径)上用纯化硅胶(60-120目)进行吸附色谱法纯化,并洗脱用200ml二氯甲烷:丙酮的混合物(1∶1,v / v)。农药通过配备〜(63)Ni电子捕获检测器(ECD)的GC和装有100%二甲基聚硅氧烷的BP色谱柱(内径30 m x 0.025 mm)进行评估。通过回收实验在各自的加标水平下测定的准确度,精密度和方法LOQ(定量限)范围为0.0018-0.0072 ug / g,回收率≥85%。检测限(LOD)为0.0005-0.0012。标准偏差的范围是0.0006-0.0018,而RSD的百分比范围是2.74-13.47。在0.001 -0.45μg/ ml的范围内获得了良好的校准曲线线性(至少r〜2≥0.99)。检出限,平均回收率%和相对标准偏差%的数据表明,该方法可用于评估马铃薯中研究的所有九种杀虫剂。

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