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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-SFOHPLC)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:20μL十一醇作为萃取剂,2μL 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2.8μg/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。
A method of surfactant-assisted-coagulation-floating dispersion-liquid-liquid microextraction-high performance liquid chromatography (SA-DLLME-SFOHPLC) was developed for the determination of four kinds of triamcinolone, atrazine, Methods for the analysis of oxazine herbicides residues. The effects of extractant type, extractant and surfactant volume, extraction time and salt effect on extraction efficiency were investigated. The optimal extraction conditions were as follows: 20μL undecyl alcohol as extractant, 2μL 0.25g / L Tween -20 aqueous solution as a dispersant, the extraction time was 10 min, the concentration of sodium chloride was 250 g / L. The results showed that the linear range of simazine, atrazine, terbuthyrin and prometryn was 0.008-5 mg / L with the detection limits of 2.4, 1.8, 2.0 and 2.8 μg / L, respectively. The enrichment factor was 24.5 ~ 32.4 between. The recoveries of simazine, atrazine, terbuthylazine and prometryn in the wines ranged from 84% to 102% with the relative standard deviations (n = 5) at 0.008, 0.08 and 2.4 mg / ) Between 2.1% ~ 6.9%. The method can be used for the determination of the wine simazine, atrazine, terbuthyrin and prometryne residues.