李敏青, 安文佳, 李菊, 王岚, 庄嘉, 何曼莉. Determination of 19 Pesticides Residues in Eggs by Gas Chromatography with Solid Phase Extraction[J]. 2020, 39(4): 520-525.DOI: doi:10.3969/j.issn.1004-4957.2020.04.014.
建立了QuEChERS及固相萃取净化技术结合气相色谱法测定禽蛋中19种农药(联苯菊酯、甲氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、敌敌畏、甲胺磷、乙酰甲胺磷、二嗪磷、乐果、甲基嘧啶磷、毒死蜱、杀螟硫磷、丙溴磷、氟虫腈、氟甲腈、氟虫腈硫醚及氟虫腈砜)残留的分析方法。蛋液样品经乙腈及QuEChERS提取盐包提取后,采用石墨化碳黑(GCB)吸附剂和十八烷基硅烷键合硅胶(C18)SPE小柱净化,以Agilent DB-1701(30 m×0.32 mm
A gas chromatographic(GC) method based on QuEChERS extraction salt package and solid phase extraction was established for the determination of 19 pesticides residues
i.e.bifenthrin
fenpropathrin
permethrin
cypermethrin
fenvalerate
deltamethrin
dichlorvos
methamidophos
acephate
diazinon
dimethoate
pirimiphos-methyl
chlorpyrifos
fenitrothion
profenofos
fipronil
fipronil-desulfinyl
fipronil sulfide and fipronil sulfone in eggs.The sample was extractd with acetonitrile and QuEChERS extraction salt package
and then purified with GCB adsorbent and C18 SPE.The analytes were separated on an Agilent DB-1701(30 m×0.32 mm
0.25 μm) polarity capillary column
then detected by GC with FPD detector and ECD detector
and quantified by external standard method.Results showed that there were good linear relationships for 19 pesticides in their respective concentration ranges
with correlation coefficients(r2) not less than 0.999 3.The recoveries at three spiked levels of low
meddle and high ranged from 78.6% to 105%
with relative standard deviations(n=6) of 1.6%-93%.The limits of detection(LOD
S/N=3) and limits of quantitation(LOQ
S/N=10) were in the ranges of 0.138-8.33 μg/kg and 0.461-27.8 μg/kg
respectively.With the advantages of simplicity
good separation
reliability and stability
the established method could meet the requirements for determination of pesticides multi residues in eggs.