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联用高效液相色谱-气相色谱法测定生物基质中的农药残留

Coupled high-performance liquid chromatography-gas chromatography for the determination of pesticide residues in biological matrices.

作者信息

Mostert I A, Ramsteiner K A

机构信息

Ciba-Geigy, Agricultural Division AG 2.53, Basle, Switzerland.

出版信息

J Chromatogr. 1989 Aug 30;477(2):359-65. doi: 10.1016/s0021-9673(01)89644-8.

Abstract

A fully automated high-performance liquid chromatography-gas chromatography (HPLC-GC) network is described. A ten-port valve set up as a loop type LC-GC interface allowed the transfer of large LC effluent fractions into the gas chromatograph by concurrent solvent evaporation. The system performed highly efficient sample enrichment and clean up by LC and on-line GC separation with sensitive electron-capture detection. The efficiency of the system was demonstrated by application to the trace analysis of N-(3-chloro-2,6-dimethylphenyl)-N-(2-oxotetrahydrofuranyl)-2-me thoxyacetamide (CGA 80000) in various crops and soil samples. The residue level determined was 0.02 mg/kg for crop samples and 0.01 mg/kg for soil samples. The relative standard deviations of the calibration graphs were in the range 2-5%; the mean recovery was greater than 85%.

摘要

本文描述了一种全自动高效液相色谱-气相色谱(HPLC-GC)联用系统。一个设置为环路型液相色谱-气相色谱接口的十通阀,通过同时进行溶剂蒸发,可将大量液相色谱流出物馏分转移至气相色谱仪中。该系统通过液相色谱进行高效的样品富集和净化,并通过灵敏的电子捕获检测进行在线气相色谱分离。通过将该系统应用于各种作物和土壤样品中N-(3-氯-2,6-二甲基苯基)-N-(2-氧代四氢呋喃基)-2-甲氧基乙酰胺(CGA 80000)的痕量分析,证明了该系统的有效性。所测定的作物样品残留水平为0.02 mg/kg,土壤样品为0.01 mg/kg。校准曲线的相对标准偏差在2-5%范围内;平均回收率大于85%。

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