QuEChERS-DLLME-高效液相色谱法测定蔬菜中溴虫腈和氟虫腈残留.pdfVIP

254 2014， 协1.35， No.24 ※分析检测 画自副事 QuEChERS-DLLME-高效液相色谱法测定 蔬菜中澳虫睛和氟虫腊残留 自宝清，李美萍，张生万* (山西大学生命科学学院，山西太原 03(削6) 摘 要z 建立同时检测蔬菜中澳虫睛和氟虫睛残留的QuEChERS-分散液液微萃取.高效液相色谱方法。样品用乙睛 溶液提取，硫酸缓和氯化铀盐析后，加入N-丙基乙二胶和石墨化碳吸附净化，分散液液微萃取富集，用SunFire-C l8 反相色谱柱分离，以甲醇和水作为流动相梯度洗脱，二极管阵列检测器进行测定，外标法定量。并考察萃取剂和分 2 散剂的类型及体积和萃取时间对萃取效率的影响。该方法在3.0-460μ.gIkg范围内线性关系良好，相关系数 (R ) 不小于0.9986，检测限0.70-0.86μ.gIkg. 3 个不同加标水平的平均回收率为90.5%-108.5%。相对标准偏差小于 10%. 结果表明，该方法简便、准确、并且成本较低，适用于蔬菜中澳虫睛和氟虫腊农药残留的测定。 关键词:澳虫腊:氟虫睛; QuEChERS; 分散液液微萃取:高效液相色谱 Determination of Chlorfenapyr and Fipronil Residues in Vegetables by QuEChERS Combined with Dispersive Liquid-liquid Microextraction and High Performance Liquid Chromatography BAI Bao-qing, LI Mei-ping , ZHANG Sheng-wan* (College of Life Sciences, Shanxi University , Tai沪Jan 03创X后， China) Abstract: A method was develo严d for simultaneous determination of the residues of chlorfenapyr and fipronil in vegetables using QuEChERS combined with dispersive liquid-liquid rnicroextraction and high performance liquid chromatography. The sample was extracted with a臼ωnitrile， salted out wi伽 MgS0 and NaCl , cleaned up with 凡propyl ethylenediarnine 4 (PSA) and graphitized carbon, and concentrated by dispersive liquid-liquid rnicroextraction (DLLME) before being analyzed by HPLC. The separation of the target compounds was performe