Wang Jiabin, Zhao Qi, Jiang Nan, Li Wenbang, Chen Li, Lin Xucong, Xie Zenghong, You Lijun, Zhang Qiqing
Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou, 350002, China.
Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou, 350002, China.
J Chromatogr A. 2017 Feb 17;1485:24-31. doi: 10.1016/j.chroma.2017.01.027. Epub 2017 Jan 10.
A novel urea-formaldehyde (UF) monolithic column has been developed and exploited as a sorbent for hydrophilic in-tube solid-phase microextraction (in-tube SPME) of aminoglycosides (AGs). Because of the innate hydrophilicity, UF monolith showed high extraction efficiency towards these hydrophilic analytes. The adsorption capacities for target compounds dissolved in water/ACN (1:1, v/v) were in the range of 5.18-7.36μg/cm. Due to the lack of a chromophore, evaporative light scattering detector (ELSD) was selected as the detector for AGs, and coupled with the online in-tube SPME-HPLC system. Several factors of the online system, such as trifluoroacetic acid (TFA) and ACN percentage in the sampling solution, ionic strength in the sample solution, elution volume, sampling and elution flow rate, were optimized with respect to the extraction efficiencies. Under the optimized conditions, the limits of detection (LODs) of streptomycin, tobramycin and neomycin were discovered in the range of 3.0-5.2μg/kg. The recoveries were ranged from 82.1 to 96.7% with relative standard deviations (RSDs) of 2.3-5.1% (n=4) at spiking levels of 50, 200 and 500μg/kg, respectively. The excellent applicability of the UF monolithic column was examined by the determination of streptomycin in practical tilapia samples, which showed the potential advantages for the analysis of polar analytes in complicated samples.
一种新型脲醛（UF）整体柱已被开发并用作氨基糖苷类（AGs）亲水型管内固相微萃取（管内SPME）的吸附剂。由于其固有的亲水性，UF整体柱对这些亲水分析物表现出高萃取效率。溶解于水/乙腈（1:1，v/v）中的目标化合物的吸附容量在5.18 - 7.36μg/cm范围内。由于缺乏发色团，选择蒸发光散射检测器（ELSD）作为AGs的检测器，并与在线管内SPME - HPLC系统联用。针对萃取效率对在线系统的几个因素进行了优化，如采样溶液中的三氟乙酸（TFA）和乙腈百分比、样品溶液中的离子强度、洗脱体积、采样和洗脱流速。在优化条件下，链霉素、妥布霉素和新霉素的检测限（LODs）在3.0 - 5.2μg/kg范围内。在加标水平分别为50、200和500μg/kg时，回收率在82.1%至96.7%之间，相对标准偏差（RSDs）为2.3%至5.1%（n = 4）。通过测定实际罗非鱼样品中的链霉素，考察了UF整体柱的优异适用性，这显示了其在复杂样品中分析极性分析物的潜在优势。
