Fe 3O 4-COOH纳米材料对大肠杆菌菌株水平的指纹峰确定

通过合成Fe ₃O ₄COOH纳米颗粒提高MALDI-TOF MS对大肠杆菌菌株水平的鉴别，并利用Fe ₃O ₄-COOH纳米对大肠杆菌K-12和大肠杆菌DSM 30083T裂解液中的菌体蛋白进行富集，不仅增加MALDI-TOF MS检测的分辨率和灵敏性，而且可以大大增加大肠杆菌菌株水平的指纹峰，根据实验结果，大肠杆菌K-12有4个匹配的指纹峰，而大肠杆菌DSM 30083T获得8个指纹峰，从而提高MALDI-TOF MS对大肠杆菌菌株水平的鉴别。     

基于新型金属有机框架模拟酶的电化学检测食品胆固醇体系的构建

基于金属有机框架具有模拟酶的特性,构建实时检测胆固醇电化学传感器。采用自组装的方法制备出新型的复合金属有机框架模拟酶(Fe₃O₄@Au/MOF)纳米粒子,其兼具了Fe₃O₄磁性粒子的可回收特点以及金纳米粒子的加速电子转移等优点。并利用红外光谱、透射电子显微镜以及X射线光电子能谱对制备成功的Fe₃O₄@Au/MOF的结构和形貌进行表征。借助Fe₃O₄@Au/MOF的类过氧化物酶双重催化性能使胆固醇氧化为胆甾烯三酮和H₂O₂,而H₂O₂在其进一步的催化下产生的具有氧化活性的羟基自由基可促进3,3′,5,5′-四甲基联苯胺发生氧化还原反应,进而增加了体系中电荷的移动。根据电信号的响应情况, 从而实现对胆固醇的快速定性和高效定量的检测。研究结果表明,采用循环伏安法测得优化检测体系为:反应温度为 50℃,Fe₃O₄@Au/MOF 添加量为0.0125g,扫描速率为0.10V/s,缓冲溶液pH=4；当胆固醇浓度处于0.001~1.500mmol/L时呈现良好的线性关系,线性回归方程为y=20.6401x+4.7722,R²=0.9956,最低检测限为2.7μmol/L；且检测体系具有良好的回收率和抗干扰性,在食品分析和生化分析等方面具有良好的应用前景。     

功能性乙基纤维素复合微球的制备及性能

将聚N-异丙基丙烯酰胺、Fe₃O₄纳米颗粒和染料4-甲胺基-9-烯丙基-1,8-萘酰亚胺与乙基纤维素溶液共混,利用高压静电喷雾技术一步法制得兼具温敏性、磁性和荧光性的乙基纤维素复合微球。结果表明,制备的乙基纤维素复合微球平均粒径在亚微米级,Fe₃O₄纳米颗粒的添加提高了复合微球的骨架强度和改善了微球形貌。当温度超过聚N-异丙基丙烯酰胺的低临界溶解温度时,乙基纤维素复合微球的平均粒径减小,表现出温敏性；基于微球的温敏响应,乙基纤维素复合微球表现出与染料溶液相反的温致荧光增强性能。振动样品磁强计分析结果表明,乙基纤维素复合微球具有良好的超顺磁性。     

来源于Anoxybacillus sp. SK3-4普鲁兰酶PulASK的固定化及酶学性质研究

普鲁兰酶在淀粉加工、多糖制备以及啤酒酿造等领域有着广泛应用。然而,该酶游离下催化产物需分离纯化和本身不可再生限制了其工业应用。磁性纳米材料具有可重复使用、磁回收性质和比表面积大等特点,有助于解决游离酶的工业化应用难题。作者将源于LAnoxybacillus sp. SK3-4的普鲁兰酶PulASK固定在纳米磁性材料Fe₃O₄@Histidine上以制备固定化酶复合体：Fe₃O₄@Histidine/PulASK,测定固定化酶的酶学性质和动力学参数。结果显示,与游离酶PulASK相比,固定化酶Fe₃O₄@Histidine/PulASK的最适反应温度由60 ℃提高到65 ℃,最适pH与游离PulASK相同;在60 ℃,pH 6.0下孵育7 h,固定化酶残余酶活为62%,而游离酶的仅为30%。分析酶动力学数据可知,在60 ℃,pH 6.0的情况下,游离酶PulASK的K_m为4.7 mmol/L,为Fe₃O₄@Histidine/PulASK的1.47倍;Fe₃O₄@Histidine/PulASK的k_cat值是350 s^-1,与PulASK的k_cat值相当,Fe₃O₄@Histidine/PulASK的k_cat/K_m是PulASK的1.57倍;并且Fe₃O₄@Histidine/PulASK在重复使用9次后,活力仍保持50%以上。与PulASK相比,Fe₃O₄@Histidine/PulASK具有良好的热稳定性且可重复使用,具有潜在应用于食品工业的价值。     

基于Fe3O4@C/\[BSMIM\]HSO4/GCE传感器检测铅离子

目的：采用Fe₃O₄@C/\[BSMIM\]HSO₄/GCE对水中的铅离子进行定量分析。方法：在四氧化三铁（Fe₃O₄）的基础上,制备了具有核壳结构的Fe₃O₄@C纳米复合材料,并复合1-甲基-3-丁磺酸基咪唑硫酸氢盐 （\[BSMIM\]HSO₄）离子液体,以玻碳电极（Glassy carbon electrode,GCE）为载体,制备了Fe₃O₄@C/\[BSMIM\]HSO₄/GCE,并利用其对饮用水中铅离子进行定量分析。结果：Fe₃O₄@C具有良好的导电性和分散性,Fe₃O₄@C/\[BSMIM\]HSO₄/GCE具有较好的电化学稳定性和电催化活性。利用Fe₃O₄@C/\[BSMIM\]HSO₄/GCE对饮用水中铅离子进行定量分析,铅离子浓度与峰电流在0.1～80.0 μg/L内呈良好的线性关系,R²=0.999 5,检出限为0.038 μg/L （S/N=3）,检出限较低,其加标回收率在97.60%～100.93%,回收效果较好,准确度较高。且该传感器重复性较好,连续差分脉冲扫描10次其相对标准偏差为2.446%。结论：该方法简单、快捷、可靠,为饮用水中铅离子的检测分析提供了一种新的解决方案。     

Al2O3负载ZnO催化臭氧氧化处理造纸废水的研究

将ZnO负载在Al₂O₃上，制备用于催化臭氧降解造纸废水中有机物的催化剂（Al₂O₃@ZnO）；采用场发射扫描电子显微镜（SEM）和X射线衍射仪（XRD）对Al₂O₃@ZnO催化剂进行物相分析；研究了造纸废水的初始pH值、反应时间和催化剂用量对Al₂O₃@ZnO催化臭氧氧化处理造纸废水效果的影响；并进行了自由基捕集剂叔丁醇实验，以探讨降解造纸废水中有机物的主要因素。结果表明，本研究成功制备了具有良好催化性能的Al₂O₃@ZnO催化剂；在造纸废水初始pH值为11、催化剂用量为2.0 g/L、反应时间为60 min的条件下，Al₂O₃@ZnO催化剂对造纸废水中COD_Cr的去除率可达到84.6％，与单独使用臭氧氧化方法相比，COD_Cr去除率明显提高，且COD_Cr的动力学降解反应遵循准一级动力学方程；叔丁醇的实验结果表明，在Al₂O₃@ZnO催化臭氧氧化处理造纸废水有机物的过程中，羟基自由基是降解废水有机物的主要因素。     

磁性疏水性纤维素纳米纤丝气凝胶的制备及性能研究

以TEMPO氧化法制备的纤维素纳米纤丝（CNF）为原料制备CNF气凝胶,随后采用Fe₃O₄纳米粒子和十六烷基三甲氧基硅烷（HDTMS）对其进行改性制得磁性疏水性CNF气凝胶,并对其疏水性能、磁性、吸附性及其他各项性能进行表征。结果表明,交联剂N,N-亚甲基双丙烯酰胺（MBA）可提高CNF之间的结合强度,使气凝胶结构更加稳定、不易被破坏。制备得到的气凝胶密度和孔隙率分别为0.015 g/cm³和99.02%,其水接触角可达133°,表现出优异的超疏水性,吸附倍率最高可达145 g/g（机油）;同时,添加Fe₃O₄纳米粒子使气凝胶具备较好的磁响应性能,有利于气凝胶的后期回收。     

纳米TiO2胶体光催化-磁絮凝回收深度处理造纸废水

以纳米TiO₂（Nano-TiO₂）为光催剂、Fe₃O₄/SiO₂（FS）为磁性絮凝剂,提出了一种通过调节pH值来实现Nano-TiO₂磁絮凝回收及解絮凝释放的回收再利用系统;研究了FS/Nano-TiO₂质量比和相同质量比下Nano-TiO₂浓度对系统絮凝性能的影响,考察了造纸废水预处理方式对Nano-TiO₂光催化-磁絮凝回收循环光降解性能的影响。结果表明,FS/Nano-TiO₂质量比越大或相同质量比下Nano-TiO₂浓度越高,两者形成的FS/Nano-TiO₂絮凝体的沉降速率越快,越有利于Nano-TiO₂的磁絮凝回收;经浓度为0.6 g/L Nano-TiO₂絮凝处理后的造纸废水（SBR-T）在光催化降解180 min后,其COD_Cr、固体悬浮物、浊度及色度分别下降了89.2%、98.2%、99.3%和99.3%,基本实现造纸废水的深度处理;相较于离心处理的造纸废水（SBR-C）的光催化降解性能（下降了25.2%）,SBR-T的光催化降解性能仅下降了11.4%,表明预先去除废水中的固体悬浮物可减少回收再利用过程中Nano-TiO₂的流失,使系统保持较高的降解效率。     

电Fenton技术深度处理造纸废水

采用电Fenton技术深度处理二级生化后的造纸废水,以色度去除率和COD去除率为主要考察指标,研究不同因素对造纸废水深度处理效果的影响。反应的最佳条件为：反应时间120 min、初始pH值=3、电压12 V、Fe²⁺浓度0.8 mmol/L、H₂O₂浓度0.8 mmol/L、极板间距10 cm、电解质Na₂SO₄浓度6 g/L。最佳反应条件下,电Fenton法对造纸废水的色度去除率和COD_Cr去除率分别达到89.5%和68.4%。动力学分析表明,电Fenton技术对造纸废水COD的降解符合一级反应动力学规律,一级反应速率常数为k=0.2072 min^-1。     

改性方法对辣木籽壳生物炭吸附亚甲基蓝的影响

目的：探究不同工艺条件所制备的辣木籽壳生物炭对亚甲基蓝的吸附性能。方法：以辣木籽壳为原料,采用超声辅助碳酸钾—Fe₃O₄共浸渍热解和KOH浸渍—1 000 ℃高温热解两种方法分别制备磁性辣木籽壳生物炭（Fe₃O₄-MOS）和改性辣木籽壳生物炭（KOH-MOS）,并用XRD、SEM和FTIR对样品表面物化性质进行表征。在此基础上,通过平衡吸附法测定两种生物炭对溶液中亚甲基蓝（MB）的吸附特性,并用动力学、热力学和等温吸附模型分析对MB的吸附机理。结果：在试验所探究的条件下,Fe₃O₄-MOS和KOH-MOS对MB的吸附效率接近100%,且由Langmuir模型所得到最大吸附量分别为116.83,99.37 mg/g。结论：两种材料对MB的吸附是一个自发吸热熵增、化学吸附为主的过程。Fe₃O₄-MOS和KOH-MOS分别展现出了良好的磁分离能力和吸附能力。     

Dispersed synthesis of uniform Fe3O4 magnetic nanoparticles via in situ decomposition of iron precursor along cotton fibre for Sudan dyes analysis in food samples

ABSTRACT

Fe₃O₄ magnetic nanoparticles, with a negative charge surface, are known to have efficient adsorbent properties, but they tend to be agglomerated into larger aggregates or flocs, which can cause loss of specific area. The addition of cotton fibre, as a stabiliser in preparation of the Fe₃O₄ nanoparticles, is able to efficiently reduce particle aggregation, and thus, effective particle size, resulting in much greater specific surface area and adsorption sites. Fe₃O₄ nanoparticles synthesis was accomplished by in situ high-temperature decomposition of the precursor ferric ion in the presence of cotton fibre and ethylene glycol solvent. The morphology of Fe₃O₄ nanoparticles was characterised by field emission scanning electron microscopy and X-ray diffraction, which confirmed that the magnetic nanoparticles are highly dispersed. These Fe₃O₄ nanoparticles were used for clean-up and pre-concentration of Sudan dyes in chilli and hot red sauces, prior to their determination by capillary liquid chromatography diode array detection. A comparative study of analyte pre-concentration was conducted with magnetic nanoparticles prepared with and without cotton fibre showing that both solid phases adsorb the analytes, but higher recoveries were obtained when using cotton fibre which therefore was selected for extraction of Sudan dyes.     

Magnetic Wood-based Superhydrophobic Aerogel for Efficient Oil-Water Separation

The fabrication of directionally driven oil-water separation materials has great significance for the removal of oil spills and organic pollutants. In this study, an oil-water separation aerogel capable of directionally adsorbing oil was designed using an anisotropic wood aerogel with a layered structure and a top-down fabrication strategy. Specifically, a magnetic wood-based superhydrophobic aerogel (methyltrimethoxysilane (MTMS)/Fe₃O₄ wood aerogel) was developed through the in situ co-precipitation of Fe₃O₄ nanoparticles and chemical vapor deposition. Owing to its highly porous structure, lipophilicity, hydrophobicity (water contact angle of 160°), and high compressibility, the MTMS/Fe₃O₄ wood aerogel exhibits excellent oil-water separation performance and compression cycle stability. Additionally, the Fe₃O₄ endows the material with excellent magnetic and photothermal conversion capabilities. These excellent properties make MTMS/Fe₃O₄ wood aerogel a promising recyclable and sustainable oil-water separation material.     

Surfactant-Alumina-Coated Magnetic Nanoparticles as an Efficient Aldehydes Adsorbent Prior Their Determination by HPLC

Separation and determination of trace levels of low-molecular weight aldehydes are very important from water suppliers’ point of view. Modified magnetic nanoparticles can be used for this propose. Alumina-coated magnetic nanoparticles modified with sodium dodecyl sulfate (SDS/Al₂O₃/Fe₃O₄) are used for extraction of formaldehyde (FA) and acetaldehyde (AA) from drinking water samples. In this manner, the aldehydes were converted to their corresponding hydrazones by the reaction with 2,4-dinitrophenylhydrazine (DNPH). After preconcentration, the HPLC technique was used for the determination of the aldehydes and the results were compared with the commercial C₁₈ solid-phase extraction (SPE) columns. The results showed that the extraction with SDS/Al₂O₃/Fe₃O₄ is more efficient and faster than the commercial columns. A very good repeatability (RSD was 3.3 and 2.4% for FA and AA, respectively, n = 7, C = 50 ppb) was obtained. Linear regression analysis indicated that the responses for two investigated compounds were linear over about two orders of magnitude above the LOD (LOD was 3.6 ppb for FA and 3.2 ppb for AA), with correlation coefficients >0.9990. Determination of FA and AA in tap water and various brands of bottled waters were carried out using the modified nanoparticles. Based on the obtained results, the aldehyde content of the commercial bottled waters was particularly apparent after exposure to direct sunlight.     

Dispersive Liquid–Liquid Microextraction Followed by Magnetic Solid-Phase Extraction for Determination of Four Parabens in Beverage Samples by Ultra-performance Liquid Chromatography Tandem Mass Spectrometry

In this study, a two-step extraction technique was developed for extraction and preconcentration of parabens from beverage samples using ionic liquid dispersive liquid–liquid microextraction (IL-DLLME) and magnetic solid-phase extraction (MSPE). In this IL-DLLME followed by MSPE method, ionic liquid (IL, 1-octyl-3-methylimidazolium hexafluorophosphate) formed hydrophobic microdroplets in beverage samples as an extractant of parabens; after the IL-DLLME process was completed, graphene modified Fe₃O₄ nanoparticles (Fe₃O₄@G) were placed to adsorb and isolate IL from the sample solution. After the supernatant was carefully moved, acetonitrile was added to elute the IL containing parabens from Fe₃O₄@G. The experimental variables affecting the extraction procedure have been systematically studied. Under optimal conditions, the detection limits were less than 1.53 ng/mL and the linear detection ranges were 2–500 ng/mL (R ² ≥ 0.998) for these analytes. The recoveries for spiked samples were 58.8–89.2% and satisfactory precision (RSD ≤ 4.8%) were obtained.     

基于共价有机骨架-MSPE-HPLC-UV法测定多环芳烃

通过一种简易的方法制备磁性共价有机骨架材料(Fe_3O_4@COF-SCU1),用于磁性固相萃取(MSPE)大红袍茶汤中8种多环芳烃,并结合高效液相色谱—紫外(HPLC-UV)法对其进行定性定量分析。采用电子扫描显微镜、电子透射显微镜、X射线衍射、氮气等温吸附脱附、傅立叶变换红外光谱对Fe_3O_4@COF-SCU1进行表征。试验系统优化了Fe_3O_4@COF-SCU1组成、MSPE的吸附及洗脱条件,并建立多环芳烃的定性定量分析方法。在最佳操作条件下,8种多环芳烃均得到良好的线性关系,相关系数≥0.998 7。方法的检出限(LODs,S/N=3)和定量限(LOQs,S/N=10)分别为0.10～0.40,0.33～1.34ng/mL。用该方法对大红袍茶汤进行分析,加标回收率为74%～106%,相对标准偏差RSD为1.20%～8.50%。结果表明,Fe_3O_4@COF-SCU1可以简便快速地萃取分离痕量水平的多环芳烃。     

Microwave absorption characterization and wettability of magnetic nano iron oxide/recycled PET nanofibers web

This paper describes the microwave characterization and wettability of a uniform and light magnetic nanofibers web. Iron oxide nanoparticles/recycled poly (ethylene terephthalate) nanofibers web (Fe₃O₄ NPs/RPET NFs web) were fabricated from bath-sonication solution via electrospinning method. For environmental conservation and economic reasons, RPET instead of virgin material was used. After synthesizing magnetic Fe₃O₄ NPs with an average diameter of 35?nm by precipitation method using iron sulfate and sodium hydroxide, Fe₃O₄ NPs/RPET NFs web was made. The main objective of this work is to show how Fe₃O₄ NPs are able to significantly modify electromagnetic properties at X-band frequencies. Microwave characterization is based on the microwave scattering parameters measured in the X-band (8–12?GHz). Various characterization methods, including field emission-scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM), have been used to study morphologies, crystalline structure, magnetic, and wettability properties of NFs web. The saturation magnetization of the Fe₃O₄ NPs/RPET NFs web at a concentration of 5% was 2.79?emu/g. The mathematical model was estimated for magnetization, diameter and concentration by MathWorks Model Predictive Control Toolbax Software. The wettability, reflection coefficient, absorption coefficient, and EMI shielding of Fe₃O₄ NPs/RPET NFs web have been improved compared to RPET NFs web.     

Functional Magnetic Nanoparticles for Highly Efficient Cholesterol Removal

In this study, magnetic nanoparticles functionalized with carboxylated β‐cyclodextrin (CM‐β‐CD; referred to Fe₃O₄@CM‐β‐CD) were synthesized and used for the efficient removal of cholesterol from milk and egg yolk via host–guest interactions. The results of Fourier‐transform infrared, X‐ray photoelectron spectroscopy, and thermogravimetric analysis indicated that the CM‐β‐CD was successfully conjugated to the surface of Fe₃O₄, and the amount of CM‐β‐CD attached on Fe₃O₄@CM‐β‐CD was determined to be 9.164%. The X‐ray diffraction and transmission electron microscopy data revealed that the process of CM‐β‐CD coating did not result in a phase change of the Fe₃O₄, and the Fe₃O₄@CM‐β‐CD nanoparticles were determined to have an average size of about 15 nm. The results of isotherm adsorption and kinetic properties indicated that CM‐β‐CD functionalization increased the cholesterol removal efficiency, and the characteristics of cholesterol adsorption on Fe₃O₄@CM‐β‐CD were fitted well with the Langmuir adsorption model and Lagergren pseudo‐1st‐order kinetic models. Furthermore, compared with the Fe₃O₄ nanoparticles, the functionalized Fe₃O₄@CM‐β‐CD nanoparticles exhibited greater cholesterol removal efficiency, and saponification of the milk and egg yolk was found to be beneficial for the cholesterol removal; using the Fe₃O₄@CM‐β‐CD nanoparticles, 98.8% and 94.6% of the cholesterol was extracted in 1 h from saponified milk and egg yolk, respectively, and the Fe₃O₄@CM‐β‐CD nanoparticles still displayed efficient cholesterol removal after 6 reuses.     

Determination of Sulfonamides in Chicken Meat by Magnetic Molecularly Imprinted Polymer Coupled to HPLC-UV

In this work, Fe₃O₄ magnetic nanoparticles were synthesized and modified by a molecularly imprinted polymer for easy and selective extraction and determination of sulfonamides in chicken meat samples. Imprinted polymer magnetic nanoparticles were characterized by Fourier transform infrared spectroscopy, X-ray diffraction pattern, thermal analysis, and scanning electron microscope micrograph. The template was removed by methanol elution. The effective parameters on extraction and determination of sulfonamides on the sorbent such as eluent type, extraction solvent, and adsorption and desorption times were optimized. Sulfonamide separation and determination were performed by high-performance liquid chromatography–UV. The linear ranges for sulfonamides were 0.5–150 μg/L and the limits of detection were 0.1–0.5 μg/L. Relative standard deviations were within 4.3–5.4 %. The method showed good selectivity for extraction of sulfonamides in real samples.     

Rapid Determination of Trace Sulfonamides in Milk by Graphene Oxide-Based Magnetic Solid Phase Extraction Coupled with HPLC–MS/MS

A simple and rapid method based on magnetic solid-phase extraction (MSPE) combined with high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC–MS/MS) was used for the determination of 15 sulfonamides from milk samples. The extraction and cleanup used a graphene oxide-based magnetic nanocomposite (Fe₃O₄@GO) as an adsorbent. Various experimental parameters that could affect the extraction efficiencies, such as the amount of Fe₃O₄@GO, the extraction time, the ionic strength of sample solution, and the type of eluent, were investigated. Under optimized experimental conditions, good linearity was observed in the range of 2.0 to 100.0 μg L^?1 for all of the analytes, with correlation coefficients (R²) ranging from 0.994 to 0.999. The limits of detection for the method ranged between 0.02 and 0.13 μg L^?1. Mean values of the relative standard deviation of intraday and interday precision ranging from 1.0 to 7.3 % and from 1.7 to 8.1 % were obtained, respectively. The average recoveries were between 73.4 and 97.4 % at three different spiked levels. It was confirmed that the Fe₃O₄@GO nanocomposite was an effective MSPE material for use in sulfonamide analyses in milk samples.     

Determination of Estrogens in Milk Samples by Magnetic‐Solid‐Phase Extraction Technique Coupled With High‐Performance Liquid Chromatography

A magnetic‐solid‐phase extraction method coupled with high‐performance liquid chromatography and diode array detection has been developed for simultaneous determination of 3 estrogens in milk samples. In this work, Fe₃O₄ NPs were synthesized by a simple chemical co‐precipitation reaction, and the surface of Fe₃O₄ was modified with cetyltrimethyl ammonium bromide (CTAB; designed as Fe₃O₄@CTAB). The synthesized Fe₃O₄@CTAB NPs were characterized by Fourier transformed infrared spectroscopy, scanning electron microscopy, and transmission electron microscope. Fe₃O₄@CTAB NPs have high binding affinity toward estrone (E1), 17β‐estradiol (17β‐E2), and diethylstilbestrol (DES). Fe₃O₄@CTAB NPs can be easily separated from sample solutions using an external magnet due to the high super‐paramagnetic property. The separation, preconcentration procedure is fast and will be completed in 2 min. Estrogens linear dynamic ranges were achieved in the range of 10 to 1000 ng/mL with regression coefficients (R²) higher than 0.9992. The limits of detection were between 0.26 and 0.61 ng/mL. Parameters influencing the recoveries were investigated and optimized. The proposed method was used for the determination of E1, 17β‐E2, and DES in milk samples, and recoveries were ranged from 91.3% to 105.0%, with the relative standard deviations in the range of 2.7% to 4.0%.