College of Chemistry, Jilin University, Changchun 130012, China.
J Chromatogr A. 2010 Jun 25;1217(26):4241-6. doi: 10.1016/j.chroma.2010.03.031. Epub 2010 Mar 27.
Dispersive liquid-liquid microextraction (DLLME) high-performance liquid chromatography (HPLC) was developed for extraction and determination of triazines from honey. A room temperature ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate [C(6)MIM][PF(6.)], was used as extraction solvent and Triton X 114 was used as dispersant. A mixture of 175 microL [C(6)MIM][PF(6)] and 50 microL 10% Triton X 114 was rapidly injected into the 20 mL honey sample by syringe. After extraction, phase separation was performed by centrifugation and the sedimented phase was analyzed by HPLC. Some experimental parameters, such as type and volume of extraction solvent, concentration of dispersant, pH value of sample solution, salt concentration and extraction time were investigated and optimized. The detection limits for chlortoluron, prometon, propazine, linuron and prebane are 6.92, 5.84, 8.55, 8.59 and 5.31 microg kg(-1), respectively. The main advantages of the proposed method are simplicity of operation, low cost, high enrichment factor and extraction solvent volume at microliter level. Honey samples were analyzed by the proposed method and obtained results indicated that the proposed method provides acceptable recoveries and precisions.
分散液液微萃取(DLLME)-高效液相色谱(HPLC)法被开发用于从蜂蜜中提取和测定三嗪类农药。采用室温离子液体 1-己基-3-甲基咪唑六氟磷酸盐([C(6)MIM][PF(6)])作为萃取溶剂,并用 Triton X-114 作为分散剂。通过注射器将 175 μL [C(6)MIM][PF(6)]和 50 μL 10% Triton X-114 的混合物迅速注入 20 mL 的蜂蜜样品中。萃取完成后,通过离心实现相与相的分离,并用 HPLC 对沉淀相进行分析。考察并优化了一些实验参数,如萃取溶剂的类型和体积、分散剂的浓度、样品溶液的 pH 值、盐浓度和萃取时间。氯丹、保棉磷、扑灭津、敌草隆和扑灭威的检测限分别为 6.92、5.84、8.55、8.59 和 5.31 μg kg(-1)。该方法的主要优点是操作简单、成本低、富集因子高,萃取溶剂用量在微升级别。采用所提出的方法对蜂蜜样品进行了分析,结果表明该方法具有可接受的回收率和精密度。