Zhong Cheng, Chen Beibei, He Man, Hu Bin
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
J Chromatogr A. 2017 Feb 3;1483:40-47. doi: 10.1016/j.chroma.2016.12.073. Epub 2016 Dec 23.
In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples.
本研究采用共价三嗪框架-1(CTF-1)作为固相萃取(SPE)吸附剂,建立了一种SPE在线联用高效液相色谱-紫外(HPLC-UV)检测的方法,用于猪肝脏和环境水样中三种硝基咪唑类药物(包括甲硝唑、罗硝唑和二甲硝唑)的痕量分析。CTF-1具有丰富的π电子和含氮三嗪,因此能与三种目标极性硝基咪唑形成π-π相互作用和分子间氢键,萃取效率高(87%-98%)。此外,CTF-1比表面积大,有利于快速传质和低柱压,吸附/解吸动力学快。考察了影响在线SPE的几个参数,包括pH值、样品流速、样品体积、解吸试剂、洗脱流速、洗脱体积和离子强度。在最佳实验条件下,检测限(S/N=3)在0.11-0.13μg/L范围内。富集因子(EFs)在52至59倍之间(理论EF为60倍)。相对标准偏差在4.3-9.4%范围内(n=7,c=1μg/L),三种目标分析物的线性范围为0.5-500μg/L。样品通量为7个/小时。该方法成功应用于猪肝脏和环境水样中硝基咪唑类药物的分析,加标样品回收率良好。