College of Chemistry, Jilin University, Changchun, China.
J Sep Sci. 2013 Feb;36(3):585-92. doi: 10.1002/jssc.201200801. Epub 2013 Jan 9.
A green and simple method, ionic liquid-based microwave-assisted surfactant-improved dispersive liquid-liquid microextraction and derivatization was developed for the determination of aminoglycosides in milk samples. Nonionic surfactant Triton X-100 and ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate were used as the disperser and extraction solvent, respectively. Extraction, preconcentration, and derivatization of aminoglycosides were carried out in a single step. Several experimental parameters, including type and volume of extraction solvent, type and concentration of surfactant, microwave power and irradiation time, concentration of derivatization reagent, and pH value and volume of buffer were investigated and optimized. Under the optimum experimental conditions, the linearities for determining the analytes were in the range 0.4-10.0 ng/mL for tobramycin, 1.0-25.0 ng/mL for neomycin, and 2.0-50.0 ng/mL for gentamicin, with the correlation coefficients ranging from 0.9991 to 0.9998. The LODs for the analytes were between 0.11 and 0.50 ng/mL. The present method was applied to the analysis of different milk samples, and the recoveries of aminoglycosides obtained were in the range 96.4-105.4% with the RSDs lower than 5.5%. The results showed that the present method was a rapid, convenient, and environmentally friendly method for the determination of aminoglycosides in milk samples.
一种绿色简单的方法，基于离子液体的微波辅助表面活性剂改进的分散液液微萃取和衍生化，用于测定牛奶样品中的氨基糖苷类抗生素。非离子表面活性剂 Triton X-100 和离子液体 1-己基-3-甲基咪唑六氟磷酸盐分别用作分散剂和萃取溶剂。氨基糖苷类抗生素的萃取、预浓缩和衍生化在一步中进行。考察并优化了几种实验参数，包括萃取溶剂的类型和体积、表面活性剂的类型和浓度、微波功率和辐射时间、衍生化试剂的浓度以及缓冲液的 pH 值和体积。在最佳实验条件下，测定分析物的线性范围为妥布霉素 0.4-10.0ng/mL，新霉素 1.0-25.0ng/mL，庆大霉素 2.0-50.0ng/mL，相关系数范围为 0.9991-0.9998。分析物的检出限在 0.11-0.50ng/mL 之间。本方法应用于不同牛奶样品的分析，氨基糖苷类抗生素的回收率在 96.4%-105.4%之间，相对标准偏差低于 5.5%。结果表明，本方法是一种快速、方便、环保的牛奶样品中氨基糖苷类抗生素的测定方法。
