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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Aluminum based metal-organic framework-polymer monolith in solid-phase microextraction of penicillins in river water and milk samples
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Aluminum based metal-organic framework-polymer monolith in solid-phase microextraction of penicillins in river water and milk samples

机译：铝基金属-有机骨架-聚合物整料在河水和牛奶样品中青霉素的固相微萃取中

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In this study, aluminum based metal-organic framework (Al-MOF)-organic polymer monoliths were prepared via microwave-assisted polymerization of ethylene dimethacrylate (EDMA), butyl methacrylate (BMA) with different weight percentages of Al-MOF (MIL-53; 37.5-62.5%) and subsequently utilized as sorbent in solid-phase microextraction (SPME) of penicillins (penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin). The Al-MOF-polymer was characterized using Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and SEM-energy-dispersive X-ray spectroscopy (SEM-EDS) to clarify the retained crystalline structure well as the homogeneous dispersion of Al-MOF (MIL-53) in polymer monolith. The developed Al-MOF-polymer (MIL-53) monolithic column was evaluated according to its extraction recovery of penicillins. Several parameters affecting the extraction recoveries of penicillins using fabricated Al-MOF-polymer (MIL-53) monolithic column including different MIL-53 weight percentages, column length, pH, desorption solvent, and mobile phase flow rate were investigated. For comparison, different Al-based MOFs (MIL-68, CYCU-4 and DUT-5) were fabricated using the optimized condition for MIL-53-polymer (sample matrix at pH 3, 200 mu L desorption volume using methanol, 37.5% of MOF, 4-cm column length at 0.100 mL min(-1) flow rate). Among all the Al-MOF-polymers, MIL-53(Al)-polymer still afforded the best extraction recovery for penicillins ranging from 90.5 to 95.7% for intra-day with less than 3.5% relative standard deviations (RSDs) and inter-day precision were in the range of 90.7-97.6% with less than 4.2% RSDs. Meanwhile, the recoveries for column-to-column were in the range of 89.5-93.5% (<3.4% RSDs) while 88.5-90.5% (<5.8% RSDs) for batch-to-batch (n=3). Under the optimal conditions, the limit of detections were in the range of 0.06-0.26 mu g L-1 and limit of quantifications between 0.20 and 0.87 mu g L-1. Finally, the MIL-53-polymer was applied for the extraction of penicillin in river water and milk by spiking trace-level penicillin for as low as 50 mu g L-1 and 100 mu g L-1 with recoveries ranging from 80.8% to 90.9% (<6.7% RSDs) in river water and 81.1% to 100.7% (<7.1% RSDs) in milk sample, respectively. (C) 2015 Elsevier B.V. All rights reserved.
机译：在这项研究中，通过微波辅助聚合具有不同重量百分比的Al-MOF（MIL-53）的二甲基丙烯酸乙二酯（EDMA），甲基丙烯酸丁酯（BMA）来制备铝基金属-有机骨架（Al-MOF）-有机聚合物整体材料; 37.5-62.5％），随后在青霉素（青霉素G，青霉素V，奥沙西林，氯沙西林，双氯西林，纳夫西林）的固相微萃取（SPME）中用作吸附剂。使用傅里叶变换红外（FTIR）光谱，粉末X射线衍射（XRD），扫描电子显微镜（SEM）和SEM能量色散X射线光谱（SEM-EDS）表征Al-MOF聚合物，以阐明保留了良好的晶体结构以及Al-MOF（MIL-53）在聚合物整料中的均匀分散。根据青霉素的提取回收率评估开发的Al-MOF-聚合物（MIL-53）整体柱。研究了使用Al-MOF-聚合物（MIL-53）整体柱影响青霉素提取回收率的几个参数，包括不同的MIL-53重量百分比，柱长，pH，解吸溶剂和流动相流速。为了进行比较，使用MIL-53-聚合物的最佳条件（pH 3的样品基质，200μL的甲醇解吸体积，37.5％的条件）制备了不同的Al基MOF（MIL-68，CYCU-4和DUT-5）。 MOF，4-cm柱长，0.100 mL min（-1）流速）。在所有的Al-MOF聚合物中，MIL-53（Al）聚合物在一天之内仍能为青霉素提供最佳的提取回收率，范围从90.5％到95.7％，相对标准偏差（RSD）小于3.5％。精度在90.7-97.6％的范围内，而RSD不到4.2％。同时，色谱柱间的回收率在89.5-93.5％（相对标准偏差<3.4％）之间，而批次间的回收率在88.5-90.5％（相对标准偏差<5.8％）之间（n = 3）。在最佳条件下，检出限为0.06-0.26μg L-1，定量限为0.20至0.87μg L-1。最后，MIL-53聚合物通过添加痕量水平的青霉素至低至50μgL-1和100μgL-1的方式应用于河水和牛奶中的青霉素提取，回收率从80.8％至牛奶样品中河水的含量分别为90.9％（RSD <6.7％），牛奶样品的RSDs为81.1％至100.7％（RSD <7.1％）。 （C）2015 Elsevier B.V.保留所有权利。

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