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食品研究与开发:2019,40(16):135-145
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QuEChERS-VADLLME-内标法-GCMS/MS快速测定铁皮石斛中的农药残留
(绿城农科检测技术有限公司,浙江杭州310052)
Study about Rapid Analysis of Pesticide Residues in Dendrobium candidum by Application of Vortex-Asisted Dispersive Liquid-Liquid Microextraction and QuEChERS and Internal Standard Method Coupled with GC-MS/MS
(Greentown Agricultural Testing Technology Co.,Ltd.,Hangzhou 310052,Zhejiang,China)
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投稿时间:2018-10-17    
中文摘要: 建立QuEChERS-涡流辅助分散液-液微萃取(vortex-assisted dispersive liquid-liquid microextraction,VADLLME)-内标法-GC-MS/MS 快速测定铁皮石斛中的农药残留。样品经乙腈溶液提取,旋涡超声后,滤液经N-丙基乙二胺(N- propyl ethylenediamine,PSA)吸附剂、C18 吸附剂净化,净化后滤液过滤膜后取1 mL 乙腈作为分散剂,加水4 mL,用0.1 mL 四氯化碳萃取,涡旋混匀,形成乳浊液经离心后吸取下层萃取液,吹干后加外环氧七氯内标,再加正己烷定容,采用气相色谱-串联质谱仪(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定。试验对萃取、富集和净化等影响因素进行优化。试验条件优化后,各农药的富集倍数可达47倍~106倍,检出限为0.353 μg/kg~1.14 μg/kg,线性范围为 0.002 mg/kg~0.5 mg/kg,相关系数为 0.990 5~0.999 9,平均加标回收率为 77.5%~97.7%,相对标准偏差0.6%~8.4%。
Abstract:A novel method for the determination of the pesticide residue in Dendrobium candidum was developed by vortex-assisted dispersive liquid-liquid microextraction (VADLLME)and QuEChERS and Internal standard coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS).The samples were extracted by acetonitrile solution and purified by N-propyl ethylenediamine (PSA)adsorbent and C18 adsorbent after vortex ultrasound.After purification,1mL acetonitrile was used as dispersant after filtrate filtration membrane,water was added to 4 mL,0.1 mL carbon tetrachloride was extracted and the vortex was mixed,then the emulsion was centrifuged and then centrifuged to absorb the lower extraction liquid.After blow dry,added seven epoxy with internal standard,and constant volume of hexane was added.Determined of GCMS/MS.The factors affecting extraction,enrichment efficiency and purification were optimized.Under the optimized experimental conditions,the concentration of each pesticide could reach 47 times-106 times,the detection limit was 0.353 μg/kg-1.14 μg/kg,the linear range was 0.002 mg/kg-0.5 mg/kg,the correlation coefficient was 0.990 5-0.999 9,the average recovery rate was 77.5 %-97.7 %,and the relative standard deviation was 0.6%-8.4%.
文章编号:201916025     中图分类号:    文献标志码:
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