表面活性剂辅助-凝固-漂浮分散液-液微萃取-高效液相色谱法检测葡萄酒中4种三嗪类除草剂残留

建立了表面活性剂辅助-凝固-漂浮分散液-液微萃取-高效液相色谱(SA-DLLME-SFO-HPLC)法检测葡萄酒中西玛津、莠去津、特丁津和扑草净4种三嗪类除草剂残留的分析方法。考察了萃取剂的类型、萃取剂和表面活性剂的体积、萃取时间和盐效应等对萃取效率的影响，确定最佳萃取条件为:20 μL十一醇作为萃取剂，2 μL 0.25 g/L的Tween-20水溶液作为分散剂，萃取时间10 min，氯化钠的质量浓度为250 g/L。结果表明:西玛津、莠去津、特丁津和扑草净的线性范围为0.008~5 mg/L，检出限分别为2.4、1.8、2.0和2.8 μg/L，富集倍数在24.5~32.4之间。在0.008、0.08和2.4 mg/L添加水平下，西玛津、莠去津、特丁津和扑草净在葡萄酒中的回收率在84%~102%之间，相对标准偏差(n=5)在2.1%~6.9%之间。该方法可用于葡萄酒中西玛津、莠去津、特丁津和扑草净残留量的测定。

Development and application of a screening method for four kinds of triazine herbicides determination in wine samples using SA-DLLME-SFO-HPLC

A new method, using on surfactant assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplets (SA-DLLME-SFO), and high performance liquid chromatography (HPLC) has been developed for the enrichment and determination of triazine herbicides in wine samples. Various experimental parameters affecting the extraction efficiencies, such as extraction solvent, extraction solvent volume, surfactant volume, extraction time and salt concentration were investigated and optimized. The following optimized conditions:extraction solvent, 20 μL1-undecanol; dispersive solvent, 2 μL 0.25 g/L Tween-20; extraction time, 10 min; NaCl addition, 250 g/L. Under the optimized conditions, the linear ranges for simazine, atrazine, terbuthylazine and prometryn were from 0.008 to 5 mg/L. The detection limits obtained for simazine, atrazine, terbuthylazine and prometryn were 2.4, 1.8, 2.0 and 2.8 μg/L, respectively. The enrichment factor were between 24.5 and 32.4. The recoveries of the different compounds were in the range of 84%-102% with the relative standard deviations were between 2.1% and 6.9% (n=5) at the spiked levels of 0.008, 0.08 and 2.4 mg/L. The proposed method was successfully applied to the analysis of simazine, atrazine, terbuthylazine and prometryn in wine.