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沸石咪唑酯骨架-8 作为在线固相萃取吸附剂,结合高效液相色谱法测定水样和奶样中的四环素类抗生素。

Zeolite imidazolate framework-8 as sorbent for on-line solid-phase extraction coupled with high-performance liquid chromatography for the determination of tetracyclines in water and milk samples.

机构信息

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.

出版信息

J Chromatogr A. 2013 Aug 23;1304:28-33. doi: 10.1016/j.chroma.2013.06.064. Epub 2013 Jun 29.

Abstract

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%.

摘要

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。

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