摘要
建立了QuEChERS-温控离子液体分散液液微萃取结合高效液相色谱法快速检测脐橙中5种染色剂残留的分析方法。 QuEChERS前处理步骤：样品用乙腈快速提取,NaCl 和无水MgSO4除水后,经N-丙基乙二胺净化。温控离子液体分散液液微萃取步骤：QuEChERS前处理的净化液（1 mL）为分散剂,1-辛基-3-甲基咪唑六氟磷酸盐离子液体（60μL）为萃取剂,55℃水浴12 min,将目标物富集。用高效液相色谱-紫外检测器分析,检出样品用超高效液相色谱-串联质谱确证。在0.01和0.05 mg/kg的添加水平下,5种染色剂的平均回收率为70.3%～93.6%,相对标准偏差为3.5%～9.2%,定量限为1.1～2.8μg/kg。
A fast method composed of the quick, easy, cheap, effective, rugged and safe （ QuEChERS） and temperature-assisted ionic liquid dispersive liquid-liquid microextraction （ TA-IL-DLLME） sample preparation coupled with high performance liquid chromatography （ HPLC ） for the analysis of 5 dyes residues in navel orange was developed. The QuEChERS sample preparation involved the quick extraction with acetonitrile in the presence of anhydrous MgSO4 and NaCl and the purification with primary secondary amine （ PSA ） sorbent. The TA-IL-DLLME sample preparation was processed using 1 mL of the extract obtained by QuEChERS as dispersive solvent and 60 μL of 1-octyl-3-methylimidazolium hexafluorophosphate as extractive solvent under 55 ℃ of water-bath temperature and 12 min of water-bath time. The ultimate solution was detected by HPLC-UV and the contaminated sample was further confirmed by UPLC-MS/MS under multiple reactions monitoring （MRM） mode. The recoveries of five dyes were in the range from 70. 3% to 93. 6% at two spike levels of 0. 01 and 0. 05 mg/kg, the relative standard deviations （RSDs） were between 3. 5% and 9. 2% and the limits of quantification （LOQs） were between 1. 1 and 2. 8 μg/kg.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第10期1434-1440,共7页
Chinese Journal of Analytical Chemistry
基金
农业部现代农业(柑桔)产业技术体系建设专项(No.CARS-27)
重庆市自然科学基金(Nos.cstc2013jjB80009
cstc2013jcyjA0435)
中央高校基本科研业务费(No.XDJK2012C059)资助项目~~
关键词
QUECHERS
分散液液微萃取
离子液体
高效液相色谱
染色剂
Quick-easy-cheap-effective-rugged and safe method
Dispersive liquid-liquid microextraction
Ionic liquid
High performance liquid chromatography
Dyes
