Pei Miao, Huang Xiaojia
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
J Chromatogr A. 2017 Sep 29;1517:1-8. doi: 10.1016/j.chroma.2017.08.007. Epub 2017 Aug 7.
To extract tetracycline antibiotics (TAs) effectively, a new adsorbent based on poly (muconic acid-co-divinylbenzene/ethylenedimethacrylate) monolith was fabricated and used as the extraction medium of multiple monolithic fiber solid-phase microextraction (MD/MF-SPME). The effect of the fabrication parameters on extraction efficiency was studied thoroughly. Elemental analysis, infrared spectroscopy, scanning electron microscopy and mercury intrusion porosimetry were used to check the physicochemical properties of the adsorbent. Some key parameters that affect the extraction performance of MD/MF-SPME for TAs were investigated systematically. Under the optimized experimental conditions, the prepared adsorbent could effectively extract the TAs through multiple interactions. At the same time, a simple and sensitive method for monitoring trace TAs in honey samples was developed by coupling MD/MF-SPME with high-performance liquid chromatography tandem mass spectrometry detection (MD/MF-SPME-HPLC-MS/MS). The limits of detection (S/N=3) for target compounds were in the range of 7.3-17.1ng/kg. The intra-day and inter-day precision (relative standard deviations, n=4, %) at 0.5μg/kg and 20.0μg/kg spiking concentrations were 5.0-9.5% and 3.6-10.0%, respectively. The mean recoveries of the target TAs in the real honey samples were between 70.5-111.0%.
为了有效提取四环素类抗生素(TAs),制备了一种基于聚(粘康酸 - 共 - 二乙烯基苯/乙二醇二甲基丙烯酸酯)整体柱的新型吸附剂,并将其用作多整体纤维固相微萃取(MD/MF - SPME)的萃取介质。深入研究了制备参数对萃取效率的影响。采用元素分析、红外光谱、扫描电子显微镜和压汞法来检测吸附剂的物理化学性质。系统研究了一些影响MD/MF - SPME对TAs萃取性能的关键参数。在优化的实验条件下,制备的吸附剂可通过多种相互作用有效萃取TAs。同时,通过将MD/MF - SPME与高效液相色谱串联质谱检测(MD/MF - SPME - HPLC - MS/MS)联用,建立了一种简单灵敏的蜂蜜样品中痕量TAs监测方法。目标化合物的检测限(S/N = 3)在7.3 - 17.1 ng/kg范围内。在0.5μg/kg和20.0μg/kg加标浓度下,日内和日间精密度(相对标准偏差,n = 4,%)分别为5.0 - 9.5%和3.6 - 10.0%。实际蜂蜜样品中目标TAs的平均回收率在70.5 - 111.0%之间。