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Synthesis of azo-linked covalent organic polymers for pipette tip solid-phase extraction of sedative residues from animal tissues samples.
Analytical Sciences ( IF 1.6 ) Pub Date : 2023-08-16 , DOI: 10.1007/s44211-023-00406-5
Jian Jun Xiang 1 , Li Juan Yuan 1 , Qie Gen Liao 1 , Da Wen Zhang 1 , Lin Guang Luo 1
Affiliation  

Azo-linked covalent organic polymers (ACOPs) were synthesized by a simple azo reaction, with 2,2'-bis(trifluoromethyl)benzidine and 1,3,5-trihydroxybenzene as the monomers. The preparation process was mild, green, and environmental-friendly, avoiding the use of high temperature, metal catalysis, and harmful organic reagent. The obtained ACOPs were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction, and Brunauer-Emmett-Teller. With the prepared ACOPs as adsorbent, a method of pipette tip solid-phase extraction-liquid chromatography-tandem mass spectrometry detection (PTSPE-LC-MS/MS) was proposed for the analysis of target sedatives in animal tissues. Furthermore, the parameters for the extraction of five sedatives, including the amount of adsorbent, pH value, ion strength, elution solvent and volume, were investigated. Under the optimized conditions, the linear dynamic range was found from 0.1 to 10.0 μg kg-1, and the limits of detection were ranged from 0.02 to 0.1 μg kg-1. The method was assessed by the analysis of target sedatives in animal tissues, and the recoveries for the spiked pork muscle and pork liver samples were 84-102% and 83-101%, respectively. The results show that the developed method of PTSPE-LC-MS/MS with ACOPs as adsorbent is efficient for the analysis of trace sedatives in animal tissues.

中文翻译:

合成偶氮连接的共价有机聚合物,用于移液器尖端固相萃取动物组织样品中的镇静残留物。

以2,2'-双(三氟甲基)联苯胺和1,3,5-三羟基苯为单体,通过简单的偶氮反应合成了偶氮连接的共价有机聚合物(ACOPs)。制备过程温和、绿色环保,避免使用高温、金属催化和有害有机试剂。通过扫描电子显微镜、傅里叶变换红外光谱、热重分析、粉末X射线衍射和Brunauer-Emmett-Teller对所得ACOP进行了表征。以制备的ACOPs为吸附剂,提出了一种移液器吸头固相萃取-液相色谱-串联质谱检测(PTSPE-LC-MS/MS)方法用于动物组织中目标镇静剂的分析。进一步考察了5种镇静剂的提取参数,包括吸附剂用量、pH值、离子强度、洗脱溶剂和体积。在优化条件下,线性动态范围为0.1~10.0 μg kg-1,检出限为0.02~0.1 μg kg-1。通过对动物组织中目标镇静剂的分析来评估该方法,加标猪肉样品和猪肝样品的回收率分别为84-102%和83-101%。结果表明,所开发的以ACOPs为吸附剂的PTSPE-LC-MS/MS方法对于动物组织中痕量镇静剂的分析是有效的。
更新日期:2023-08-16
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