【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。更多还原

【Abstract】 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% and9. 2% and the limits of quantification(LOQs) were between 1. 1 and 2. 8 μg /kg.更多还原