植物油和乳脂肪中有机磷和有机氯农药残留的多柱固相萃取净化
Multicolumn solid-phase extraction cleanup of organophosphorus and organochlorine pesticide residues in vegetable oils and butterfat.
作者信息
Gillespie A M, Daly S L, Gilvydis D M, Schneider F, Walters S M
机构信息
U.S. Food and Drug Administration, Pesticides and Industrial Chemicals Research Center, Detroit, MI 48207, USA.
出版信息
J AOAC Int. 1995 Mar-Apr;78(2):431-7.
Diatomaceous earth columns used with reversed and normal solid phase extraction (SPE) cartridges were evaluated for the quantitative determination of a number of organophosphorus (OP) and organochlorine (OC) pesticide residues in edible vegetable oils and butterfat. An oil or fat sample (about 2 g) in hexane was passed through a diatomaceous earth (Extrelut QE) column and a C18 bonded silica (ODS) SPE cartridge, resulting in the separation of the pesticides from about 98% of the lipids. The eluate was split in half, with the first portion concentrated into acetone for the determination of OP pesticides by gas chromatography with flame photometric detection (GC-FPD). The other half was passed through an Alumina-N SPE cartridge for additional cleanup of lipid matrix to determine OC pesticides by GC with electron-capture detection (GC-ECD). Average recoveries from fortified samples were greater than 89% for the pesticides studied.
评估了与反相和正相固相萃取（SPE）小柱联用的硅藻土柱，用于定量测定食用植物油和乳脂中的多种有机磷（OP）和有机氯（OC）农药残留。将约2 g己烷中的油脂样品通过硅藻土（Extrelut QE）柱和C18键合硅胶（ODS）SPE小柱，使约98%的脂质与农药分离。洗脱液分成两半，第一部分浓缩至丙酮中，通过气相色谱 - 火焰光度检测（GC - FPD）测定OP农药。另一半通过氧化铝 - N SPE小柱进一步净化脂质基质，通过气相色谱 - 电子捕获检测（GC - ECD）测定OC农药。对于所研究的农药，加标样品的平均回收率大于89%。
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