State Key Laboratory of Medicinal Chemical Biology, Synergetic Innovation Center of Chemical Science and Engineering (Tianjin), and Research Center for Analytical Sciences, College of Chemistry, Nankai University, Tianjin 300071, China.
J Chromatogr A. 2013 Aug 23;1304:28-33. doi: 10.1016/j.chroma.2013.06.064. Epub 2013 Jun 29.
Zeolite imidazolate framework-8 (ZIF-8) was used as the novel sorbent for on-line solid-phase extraction coupled with high-performance liquid chromatography (HPLC) for the determination of oxytetracycline (OTC), tetracycline (TC) and chlorotetracycline (CTC) in water and milk samples. 390mg of ZIF-8 was packed into a stainless steel column (3cm long×4.6mm i.d.) which was mounted on the HPLC injector valve to replace the sample loop. On-line solid-phase extraction of OTC, TC and CTC was achieved by loading sample solution at a flow rate of 3.0mLmin(-1) for 10min with the aid of a flow-injection system. The extracted analytes were subsequently eluted into a C18 analytical column (25cm long×4.6mm i.d.) for HPLC separation under isocratic condition with a mobile phase (10% MeOH-20% ACN-70% 0.02molL(-1) oxalic acid solution) at a flow rate of 1.0mLmin(-1). Under optimized conditions, the developed method gave the enhancement factors of 35-61, the linearity range of 5-1000μgL(-1), the detection limits of 1.5-8.0μgL(-1), quantification limits of 5.0-26.7μgL(-1), uncertainties of 0.9-1.1μgL(-1), and the sample throughput of 4 samples h(-1). The recoveries of OTC, TC and CTC at 50μgL(-1) in water and milk samples ranged from 70.3% to 107.4%.
沸石咪唑酯骨架-8(ZIF-8)被用作新型吸附剂,用于在线固相萃取与高效液相色谱(HPLC)联用,以测定水样和奶样中的土霉素(OTC)、四环素(TC)和金霉素(CTC)。390mg 的 ZIF-8 被填充到不锈钢柱(3cm 长×4.6mm内径)中,该柱安装在 HPLC 进样阀上,以代替样品环。在流动注射系统的辅助下,以 3.0mLmin(-1)的流速加载样品溶液 10min,实现了 OTC、TC 和 CTC 的在线固相萃取。提取的分析物随后用 C18 分析柱(25cm 长×4.6mm 内径)洗脱,在等度条件下用流动相(10% MeOH-20% ACN-70% 0.02molL(-1) 草酸溶液)以 1.0mLmin(-1)的流速进行 HPLC 分离。在优化条件下,该方法的增强因子为 35-61,线性范围为 5-1000μgL(-1),检测限为 1.5-8.0μgL(-1),定量限为 5.0-26.7μgL(-1),不确定度为 0.9-1.1μgL(-1),样品通量为 4 个样品 h(-1)。在水和奶样中,50μgL(-1) 的 OTC、TC 和 CTC 的回收率在 70.3%-107.4%之间。