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Solid-phase extraction and separation of indium with P_(2)O_(4)-UiO-66-MOFs (di-2-ethylhexyl phosphoric acid-UiO-66-metal-organic frameworks)

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Journal of Environmental Sciences 2023年第5期127卷 833-843页

作者： Wan-Yi Zeng Minzhong Huang Minglai Fu Key Laboratory of Urban Pollutant Conversion Institute of Urban EnvironmentChinese Academy of SciencesXiamen 361021China University of Chinese Academy of Sciences Beijing 100049China School of Electromechanical Engineering Guangdong University of TechnologyGuangzhou 510006China Xiamen Key Laboratory of Municipal and Industrial solid Waste Utilization and Pollution Control College of Civil EngineeringHuaqiao UniversityXiamen 361021China

Compared with the traditional liquid–liquid extraction method,Solid-phase extraction agents are of great significance for the recovery of indium metal due to their convenience,free of organic solvents,and fully exposed activity.In this study,P_(2)O_(4)(di-2-ethylhexyl phosphoric acid)was chemically modified by using UiO-66 to form the Solid-phase extraction agent P_(2)O_(4)-UiO-66-MOFs(di-2-ethylhexyl phosphoric acid-UiO-66-metal-organic frameworks)to adsorb In(Ⅲ).The results show that the Zr of UiO-66 bonds with the P-OH of P_(2)O_(4) to form a composite P_(2)O_(4)-UiO-66-MOF,which was confirmed by X-ray photoelectron spectroscopy(XPS)and Fourier transform infrared spectroscopy(FT-IR).The adsorption process of indium on P_(2)O_(4)-UiO-66-MOFs followed pseudo first-order kinetics,and the adsorption isotherms fit the Langmuir adsorption isotherm model.The adsorption capabilities can reach 192.8 mg/g.After five consecutive cycles of adsorption-desorption-regeneration,the indium adsorption capacity by P_(2)O_(4)-UiO-66-MOFs remained above 99%.The adsorption mechanism analysis showed that the P=O and P-OH of P_(2)O_(4) molecules coated on the surface of P_(2)O_(4)-UiO-66-MOFs participated in the adsorption reaction of indium.In this paper,the extractant P_(2)O_(4) was modified into solid P_(2)O_(4)-UiO-66-MOFs for the first time.This work provides a new idea for the development of solid-phase extractants for the recovery of indium.

关键词： P_(2)O_(4)-UiO-66-MOFs(di-2-Ethylhexyl phosphoric acid-UiO-66-metal-organic frameworks) Solid-phase extraction Adsorption Indium(III)

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Simultaneous determination of three classes of antibiotics in the suspended solids of swine wastewater by ultrasonic extraction,Solid-phase extraction and liquid chromatography-mass spectrometry

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Journal of Environmental Sciences 2011年第10期23卷 1729-1737页

作者： Xun Pan Zhimin Qiang Weiwei Ben Meixue Chen Research Center for Eco-Environmental Sciences Chinese Academy of Sciences Beijing 100085 China

This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids （SS） of swine wastewater, including five sulfonamides, three tetracyclines and one macrolide （tiamulin）. The entire procedures for sample pretreatment, ultrasonic extraction （USE）, Solid-phase extraction （SPE）, and liquid chromatography-mass spectrometry （LC-MS） quantification were examined and optimized. The recovery efficiencies were found to be 76%-104% for sulfonamides, 81%-112% for tetracyclines, and 51%--64% for tiamulin at three spiking levels. The intra-day and inter-day precisions, as expressed by the relative standard deviation （RSD）, were below 17%. The method detection limits （MDLs） were between 0.14 and 7.14 μg/kg, depending on a specific antibiotic studied. The developed method was applied to field samples collected from three concentrated swine feeding plants located in Beijing, Shanghai and Shandong province of China. All the investigated antibiotics were detected in both SS and liquid phase of swine wastewater, with partition coefficients （logKd） ranging from 0.49 to 2.30. This study demonstrates that the SS can not be ignored when determining the concentrations of antibiotics in swine wastewater.

关键词： antibiotics swine wastewater suspended solids ultrasonic extraction Solid-phase extraction mass spectrometry

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Solid-phase extraction of trace Au(Ⅲ) with SDG and determination by the catalytic spectrophotometric method

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Rare Metals 2008年第6期27卷 560-565页

作者： LI Huizhi ZHAI Yubo School of Chemistry and Chemical Engineering Jinan University Jinan 250022 China School of Life Science Nanjing University Nanjing 210093 China

The new catalytic kinetic spectrophotometric method for Au（III） determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate （（NH4）2S2O8） with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au（Ⅲ） at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel （SDG） as a solid-phase extractant has been developed for the preconcentration and separation of Au（Ⅲ） ions. The method has been applied to the determination of trace gold with satisfactory results.

关键词： analytical chemistry catalytic kinetic spectrophotometric method Solid-phase extraction gold（Ⅲ）

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Solid-phase extraction and separation of heavy rare earths from chloride media using P227-impregnated resins

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Rare Metals 2021年第9期40卷 2633-2644页

作者： Bin Yang Suo-Zhi Wu Xin-Yu Liu Zeng-Xin Yan Yu-Xue Liu Qi-Song Li Feng-Shan Yu Jun-Lian Wang School of Civil and Resource Engineering University of Science and Technology BeijingBeijing 100083China Jiangxi Province Han’s Precious Metals Co. LtdShangrao 335500China

A Solid-phase extraction resin SIRs-P227/XAD-7 HP was prepared by impregnating extractant P227 onto macroporous resin XAD-7 HP beads. SIRs-P227/XAD-7 HP beads were characterized by Fourier transform infrared spectroscopy(FTIR) and scanning electron microscopy(SEM) equipped with energy-dispersive spectroscopy(EDS). The adsorption kinetics, particle size effect,adsorption isotherm, pH_(equilibrium)–lg D relationship(where D is distribution coefficient), desorption, adsorption selectivity for heavy rare earths, and impurity ions were studied. The results showed that the adsorption kinetics of Lu(III) on the SIRs-P227/XAD-7 HP beads fitted the Morris–Weber model best. The adsorbance decreased as the particle size increased. The pH_(equilibrium)–lg D relationship fitted well with a straight line, and the slope was 1.56. The experimental data fitted well with Langmuir adsorption.The calculated maximum adsorption capacity was23.8 mg·g^(-1), while the experimental datum was22.7 mg·g^(-1) at the given conditions. The adsorbed Lu(III)can be easily stripped by 0.1 mol·L^(-1) HCl. The adsorption selectivity of SIRs-P227/XAD-7 HP for heavy REs exhibited the following order: Lu>Yb>Tm>Er>Ho. The adjacent heavy rare earth(RE) separation factors β_(Lu/Yb),β_(Yb/Tm), β_(Tm/Er), and β_(Er/Ho)were 1.57, 3.00, 3.03, and 2.23,respectively, at liquid/solid ratio(L/S) equal to 3:20. The adsorption selectivity for impurity ions exhibited the followingorder:Fe >Lu>Tm>Zn>Mg>Ca>Ho>Co>Ni>Cu>Al.

关键词： Solid-phase extraction Solvent-impregnated resins P227 Heavy rare earths

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Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

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Rare Metals 2007年第6期26卷 541-546页

作者： MA Xiaoguo HUANG Bei CHENG Meiqing Faculty of Environmental Science and Engineering Guangdong University of Technology Guangzhou 510090 China Department of Chemical Engineering Maoming University Maoming 525000 China

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide （TiO2） as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry （CVAAS）. Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg^2＋on the dithizone-modified nanoparficles was investigated in detail. It was found that excellent adsorption ratio for Hg^2＋ could be obtained in the pH range of 7-8 with an oscillation time of 15 rain, and a 5 mL of 3.5 mol·L^-1 HCI solution could quantitatively elute Hg^2＋ from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit （30） for Hg^2＋ was calculated to be 5 ng·L^-1. The proposed method was applied to the determination of Hg^2＋ in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD （n = 5） of 2.9%-3.5%.

关键词： analytical chemistry mercury Solid-phase extraction TiO2 nanoparticle cold vapor atomic adsorption spectrometry （CVAAS）

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Simple and Sensitive Determination of Aromatic Acids in Coconut Water by g-C3N4@SiO2 Based solid-phase extraction and HPLC-UV Analysis

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Chemical Research in Chinese Universities 2018年第4期34卷 528-535页

作者： QIANGBA Gezhen ZHU Gangtian YU Qiongwei FENG Yuqi Key Laboratory of Analytical Chemistry for Biology and Medicine Ministry of Education Department of Chemistry Wuhan University Wuhan 430072 P. R. China Key Laboratory of Tectonics and Petroleum Resources Ministry of Educan'on China University of Geosciences Wuhan 430075 P. R. China

In this study, graphitic carbon nitride deposited silica（g-C3N4@SiO2） was prepared by simple pyrolysis of melamine on silica and then used as a Solid-phase extraction（SPE） sorbent for the extraction of four representative aromatic acids including benzoic acid（BA）, salicylic acid（SA）, indolyl-3-butyricacid（IBA） and naphthalene acetic acid（NAA） in coconut water（CW） samples, g-C3N4@SiO2 exhibited an excellent adsorption capacity for the four aromatic acids, which are in the concentration range of 500--558.8 gg/g. The four aromatic acids could be directly captured by g-C3N4@SiO2 from CW samples within 5 rain. Thus, a rapid, simple and effective method for the analy- sis of four aromatic acids in CW samples was developed by coupling g-C3N4@SiO2-based SPE with high performance liquid chromatography-ultraviolet（HPLC-UV） detection. The linearity of the developed method was in the range of 20--1000 ng/mL and its limit of detection was in the range of 1.9--5.7 ng/mL, which were signi- ficantly lower than those of the reported similar methods. The intra-day and inter-day precisions（based on the relative standard deviation, n=3） of the four aromatic acids were under 9.5% and 10.4%, respectively. The developed method was applied to determining the four aromatic acids in real CW samples and the spiked recoveries varied from 81.1% to 121.8%.

关键词： Aromatic acid Coconut water Solid-phase extraction Graphitic carbon nitride High-performance liquidchromatography

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A Solid-phase extraction approach for the identification of pharmaceutical–sludge adsorption mechanisms

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Journal of Pharmaceutical Analysis 2014年第2期4卷 117-124页

作者： Laurence Berthod Gary Roberts Graham A.Mills AstraZeneca Brixham Environmental Laboratory Freshwater QuarryBrixhamDevon TQ5 8BAUK School of Pharmacy and Biomedical Sciences University of PortsmouthPortsmouthHampshirePO1 2DTUK

It is important to understand the adsorption mechanism of chemicals and active pharmaceu-tical ingredients （API） on sewage sludge since wastewater treatment plants are the last barrier before the release of these compounds to the environment. Adsorption models were developed considering mostly hydrophobic API-sludge interaction. They have poor predictive ability, especially with ionisable compounds. This work proposes a Solid-phase extraction （SPE） approach to estimate rapidly the API-sludge interaction. Sludge-filled SPE cartridges could not be percolated with API spiked mobile phases so different powders were tested as SPE sludge supports. Polytetrafluoroethylene （PTFE） was selected and tested at different PTFE/sludge ratios under eight different adsorption conditions with three API ionisable compounds. The PTFE/sludge mixtures with 50% or less sludge could be used in SPE mode for API sorption studies with methanol/water liquid phases. The results gave insights into API-sludge interactions. It was found that π-π, hydrogen-bonding and charge-charge interactions were as important as hydrophobicity in the adsorption mechanism of charged APIs on sludge.

关键词： Pharmaceuticals Sewage sludge Adsorption coefficient Binding Solid-phase extraction Polytetrafl uoroethylene

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Surface molecularly imprinted polymers for Solid-phase extraction of （-）-epigallocatechin gallate from toothpaste

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Frontiers of Chemical Science and Engineering 2015年第4期9卷 467-478页

作者： Yunling Gao Ying Hu Kejian Yao State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology College of Chemical Engineering Zhejiang University of Technology Hangzhou 310032 China

Surface molecularly imprinted polymers （SMIPs） have been synthesized to selectively determine （-）-epigallocatechin gallate in aqueous media. SMIPs were prepared using a surface grafting copolymerization method on a functionalized silica gel modified with β-cyclodextrin and vinyl groups. The morphology and composition of the SMIPs were investigated by scanning electron microscopy, Fourier transform-infrared spectroscopy and thermogravimetric analysis. In addition, the molecular binding capacity, recognition properties and selectivity of the SMIPs were evaluated. The imprinted polymers were found to have a highly specific recognition and binding capacity for aqueous media which is （-）-epigallocatechin gallate in the result of the hydrophobic properties of the β-cyclodextrin and the hydrogen-bonding interactions of methacrylic acid. The SMIPs were successfully employed as Solid-phase extraction adsor- bents prior to the HPLC determination of （-）-epigallocatechin gallate in toothpaste. The HPLC analysis had a linear dynamic range of 0.5-50.0 μg·mL^-1 with a correlation coefficient of 0.9998 and the recoveries ranged from 89.4% to 97.0% with relative standard deviations less than 4.8%. The limit of detection and limit of quantification were 0.17 and 0.33 μg·mL^-1, respectively. The method provides a promising approach for the preparation of selective materials for the purification and determination of complex samples.

关键词： β-cyclodextrin （-）-epigallocatechin gallate,surface molecular imprinting Solid-phase extraction

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Comparison of liquid-liquid extraction-thin layer chromatography with Solid-phase extraction-high-performance thin layer chromatography in detection of urinary morphine

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The Journal of Biomedical Research 2011年第5期25卷 362-367页

作者： Ali Ahadi Alireza Partoazar Mohammad Hassan Abedi Khorasgani Seyed Vahid Shetab Boushehri Department of Physiology School of MedicineTehran University of Medical Sciences Department of Pharmacology School of MedicineTehran University of Medical Sciences Legal Medicine Organization of Iran Iran Department of Medical Nanotechnology School of MedicineTehran University of Medical Sciences

Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.

关键词： morphine detection liquid-liquid extraction thin-layer chromatography Solid-phase extraction highperformance thin layer chromatography

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Determination of N-Methylcarbamate Pesticides in Vegetables by Solid-phase extraction and Pressurized Capillary Electrochromatography

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Chemical Research in Chinese Universities 2007年第1期23卷 109-115页

作者： WU Xiao-ping WANG Ling XIE Zeng-hong YAN Chao CHEN Guo-nan Key Laboratory of Food Safety Analysis and Detection Technology of MOE Department of Chemistry Fuzhou University Fuzhou 350002 P. R. China Unimicro Technologies Inc. Pleasanton CA94566 USA

Capillary electrochromatography （CEC） is a hybrid technique that couples the good selectivity of high-performance liquid chromatography （HPLC） and the high separation efficiency of capillary electrophoresis （CE）. Both charged and uncharged compounds can be separated effectively using CEC. In some cases, however, the bubbles that generated in the capillary column in pure CEC performed on commercial CE instruments will cause unstable current and even disrupt the separation when the concentration of buffer is very high. By applying pressure on the electrochromatographic separation via a micro-HPLC pump, pressurized capillary electrochromatography （ pCEC ） combines two driving factors of the electroosmotic flow （EOF） and the pressure flow, thereby increasing the speed and the selectivity of separation and suppressing the bubble formation. Moreover,

关键词： Pressurized capillary electrochromatography N-Methylcarbamate Pesticide Solid-phase extraction

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