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基于金属有机骨架的分子印迹固相分散法分析奶粉中的四环素类药物,采用超高效液相色谱-串联质谱法。

Analysis of tetracyclines from milk powder by molecularly imprinted solid-phase dispersion based on a metal-organic framework followed by ultra high performance liquid chromatography with tandem mass spectrometry.

机构信息

Department of Chemistry, College of Science, Northeast Forestry University, Harbin, China.

Center of Disease Control of Heilongjiang Province, Harbin, China.

出版信息

J Sep Sci. 2018 Jun;41(12):2604-2612. doi: 10.1002/jssc.201701514. Epub 2018 May 2.

Abstract

A novel molecularly imprinted polymer that could selectively recognize tetracyclines in milk powder was synthesized using a metal-organic framework as a support material, tetracycline as template molecule, and 3-aminophenylboronic acid as a functional monomer and a cross-linking agent. The novel molecularly imprinted polymer was characterized by Fourier transform infrared spectrometry, transmission electron microscopy, X-ray diffractometry, thermogravimetric analysis, and N adsorption/desorption measurements. The adsorption isotherms, adsorption kinetics, adsorption thermodynamics, and selective adsorption experiments of the novel molecularly imprinted polymer to tetracycline were also studied. The novel molecularly imprinted polymer was used as dispersant of matrix solid-phase dispersion to extraction tetracyclines. After that, the tetracyclines extracted from milk powder were determined by ultra high performance liquid chromatography with tandem mass spectrometry. Under the optimal conditions, the detection limits of tetracyclines were 0.217-0.318 ng/g. The relative standard deviations of intra- and interday precision ranged from 3.8 to 6.9% and from 2.8 to 7.4%, respectively. In all three concentration levels (1.0, 10, 50 ng/g), the recoveries of tetracyclines ranged from 84.7 to 93.9%. The method was successfully applied to the determination of tetracyclines in milk powder.

摘要

采用金属有机框架作为支撑材料,以四环素为模板分子,3-氨基苯硼酸为功能单体和交联剂,合成了一种可选择性识别奶粉中四环素的新型分子印迹聚合物。通过傅里叶变换红外光谱、透射电子显微镜、X 射线衍射、热重分析和 N 吸附/解吸测量对新型分子印迹聚合物进行了表征。还研究了新型分子印迹聚合物对四环素的吸附等温线、吸附动力学、吸附热力学和选择性吸附实验。将新型分子印迹聚合物用作基质固相分散的分散剂,提取奶粉中的四环素。然后,采用超高效液相色谱-串联质谱法测定。在最佳条件下,四环素的检测限为 0.217-0.318ng/g。日内和日间精密度的相对标准偏差分别为 3.8-6.9%和 2.8-7.4%。在三个浓度水平(1.0、10、50ng/g)下,四环素的回收率均在 84.7-93.9%之间。该方法成功应用于奶粉中四环素的测定。

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