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气相色谱法测定狭叶松果菊(菊科)根中尿嘧啶类除草剂的含量

Gas chromatographic method for determination of uracil herbicides in roots of Echinacea angustifolia Moench (Asteraceae).

作者信息

Tekel J, Tahotná S, Vaverková S

机构信息

Faculty of Pharmacy, Comenius University, Bratislava, Slovakia.

出版信息

J Pharm Biomed Anal. 1998 Jan;16(5):753-8. doi: 10.1016/s0731-7085(97)00118-0.

Abstract

A GC/NPD method and a rapid screening TLC method were developed for the simultaneous determination of uracil herbicide residues (bromacil, lenacil, terbacil) in the roots of Echinacea angustifolia Moench (Asteraceae). The uracil herbicide residues were extracted into acetone. After evaporation of acetone from the acetone-water extract the residue was dissolved in water-methanol (5:1 v/v). Cyclohexane was used for removal of the non-polar co-extractives in the sample matrix. After separation of the cyclohexane phase the uracil herbicide residues were extracted into chloroform. This extract was purified on a Florisil column, and residues were eluted with dichloromethane-acetone (9:1, v/v). The cleaned up extract was analysed by the GC/NPD method on a capillary column DB-1 using atrazine as internal standard. A minimum recovery of 70% was attained for contamination levels of 0.02-0.40 mg kg(-1).

摘要

建立了一种气相色谱/氮磷检测器(GC/NPD)方法和一种快速筛选薄层色谱(TLC)方法,用于同时测定狭叶松果菊(菊科)根中尿嘧啶类除草剂残留(溴莠定、利谷隆、特草定)。尿嘧啶类除草剂残留用丙酮提取。从丙酮 - 水提取物中蒸去丙酮后,残渣溶于水 - 甲醇(5:1,v/v)。环己烷用于去除样品基质中的非极性共提取物。分离环己烷相后,尿嘧啶类除草剂残留用氯仿提取。该提取物在弗罗里硅土柱上净化,残留物用二氯甲烷 - 丙酮(9:1,v/v)洗脱。净化后的提取物采用GC/NPD方法在DB - 1毛细管柱上进行分析,以莠去津作为内标。对于0.02 - 0.40 mg kg⁻¹的污染水平,最低回收率达到70%。

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