Chen Huaixia, Chen Hui, Liao Lei, Ying Jun, Huang Jianlin
Ministry of Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules & College of Chemistry and Chemical Engineering, Hubei University, Wuhan 430062, China.
J Chromatogr Sci. 2010 Jul;48(6):450-5. doi: 10.1093/chromsci/48.6.450.
Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-variable wavelength detector (HPLC-VWD) was developed for extraction and determination of thiamphenicol (THA) in honey. A mixture of extraction solvent (30 microL 1,1,2,2-tetrachloroethane) and dispersive solvent (1.0 mL of acetonitrile) was rapidly injected into 5.00 mL sample solution for the formation of cloudy solution. The analyte in the sample was extracted into the fine droplets of C(2)H(2)Cl(4). After extraction, phase separation was performed by centrifugation, and the enriched analyte in the sedimented phase was determined by HPLC-VWD. Some important parameters, such as the kind and volume of extraction solvent and dispersive solvent, extraction time, sample solution pH, sample volume, and salt effect, were investigated and optimized. Under the optimum extraction condition, the method yielded a linear calibration curve in the concentration range from 3 to 2000 microg/kg for target analyte. The enrichment factors for THA was 87.9, and the limit of detection (S/N = 3) was 0.1 microg/kg. The relative standard deviation for the extraction of 10 microg/kg of THA was 6.2% (n = 6). The main advantages of DLLME-HPLC method are simplicity of operation, rapidity, low cost, high enrichment factor, high recovery, good repeatability, and extraction solvent volume at the microL level. Honey samples were successfully analyzed using the proposed method.
建立了分散液液微萃取(DLLME)结合高效液相色谱 - 可变波长检测器(HPLC - VWD)用于蜂蜜中氟苯尼考(THA)的萃取和测定。将萃取溶剂(30 μL 1,1,2,2 - 四氯乙烷)和分散溶剂(1.0 mL乙腈)的混合物快速注入5.00 mL样品溶液中形成浊液。样品中的分析物被萃取到C₂H₂Cl₄的细小液滴中。萃取后,通过离心进行相分离,沉淀相中富集的分析物用HPLC - VWD测定。研究并优化了一些重要参数,如萃取溶剂和分散溶剂的种类及体积、萃取时间、样品溶液pH值、样品体积和盐效应。在最佳萃取条件下,该方法对目标分析物在3至2000 μg/kg浓度范围内得到线性校准曲线。氟苯尼考的富集因子为87.9,检测限(S/N = 3)为0.1 μg/kg。10 μg/kg氟苯尼考萃取的相对标准偏差为6.2%(n = 6)。DLLME - HPLC方法的主要优点是操作简单、快速、成本低、富集因子高、回收率高、重复性好且萃取溶剂体积在微升水平。使用该方法成功分析了蜂蜜样品。