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Determination of selected semi-volatile organic compounds in water using automated online solid-phaseextraction with large-volume injection/gas chromatography/mass spectrometry

Yongtao LI, Christina L. MCCARTY, Ed J. GEORGE

《环境科学与工程前沿（英文）》 2011年 第5卷 第3期   页码 417-425 doi: 10.1007/s11783-011-0310-x

摘要： A rapid, sensitive, and cost-effective analytical method was developed for the analysis of selected semi-volatile organic compounds in water. The method used an automated online solid-phase extraction technique coupled with programmed-temperature vaporization large-volume injection gas chromatography/mass spectrometry. The water samples were extracted by using a fully automated mobile rack system based on x-y-z robotic techniques using syringes and disposable 96-well extraction plates. The method was validated for the analysis of 30 semi-volatile analytes in drinking water, groundwater, and surface water. For a sample volume of 10 mL, the linear calibrations ranged from 0.01 or 0.05 to 2.5μg·L , and the method detection limits were less than 0.1μg·L . For the reagent water samples fortified at 1.0μg·L and 2.0?μg·L , the obtained mean absolute recoveries were 70%–130% with relative standard deviations of less than 20% for most analytes. For the drinking water, groundwater, and surface water samples fortified at 1.0μg·L , the obtained mean absolute recoveries were 50%–130% with relative standard deviations of less than 20% for most analytes. The new method demonstrated three advantages: 1) no manipulation except the fortification of surrogate standards prior to extraction; 2) significant cost reduction associated with sample collection, shipping, storage, and preparation; and 3) reduced exposure to hazardous solvents and other chemicals. As a result, this new automated method can be used as an effective approach for screening and/or compliance monitoring of selected semi-volatile organic compounds in water.

关键词： automated solid-phase extraction     programmed-temperature vaporization     large-volume injection     gas chromatography/mass spectrometry     semi-volatile organic compounds     water analysis    

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

Yunling Gao,Ying Hu,Kejian Yao

《化学科学与工程前沿（英文）》 2015年 第9卷 第4期   页码 467-478 doi: 10.1007/s11705-015-1526-2

摘要： 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 -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 (−)-epigallocatechin gallate in aqueous media which is the result of the hydrophobic properties of the -cyclodextrin and the hydrogen-bonding interactions of methacrylic acid. The SMIPs were successfully employed as solid-phase extraction adsorbents 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 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 , 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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aniline derivatives in water samples after preconcentration with oxidized multiwalled carbon nanotubes as solid-phaseextraction disk

Hideyuki KATSUMATA, Yuta ODA, Satoshi KANECO, Tohru SUZUKI, Kiyohisa OHTA

《化学科学与工程前沿（英文）》 2012年 第6卷 第3期   页码 270-275 doi: 10.1007/s11705-012-1298-x

摘要： A sensitive and selective preconcentration method using solid-phase extraction (SPE) disk made from oxidized multiwalled carbon nanotubes (OMWCNTs), has been developed for the determination of aniline derivatives, such as 2-nitroaniline (2-NA), 4-nitroaniline (4-NA), and 2,4-dichloroaniline (2,4-DCA) in water samples. Anilines were extracted onto OMWCNT disk and then determined by high performance liquid chromatography (HPLC) with UV detector. Several parameters on the recovery of the analytes were investigated. The experimental results showed that it was possible to obtain quantitative analysis when the solution pH was 8 using 200 mL of validation solution containing 2 μg of anilines and 10 mL of acetonitrile/ethanol (8/2, v/v) as an eluent. Relative standard deviations for five determinations were 7.5% (2-NA), 6.5% (4-NA) and 3.8% (2,4-DCA) under optimum conditions. The linear range of calibration curves were 0.5 ng·mL to 15 ng·mL for each analyte with good correlation coefficients. The detection limits (3S/N) of 2-NA, 4-NA and 2,4-DCA were 30 pg·mL , 31 pg·mL and 26 pg·mL , respectively. Our method was successfully applied to the determination of aniline compounds in river water sample with high precision and accuracy.

关键词： aniline determination     solid-phase extraction     oxidized multiwalled carbon nanotubes     water sample     HPLC-UV    

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Simultaneous analysis of five taste and odor compounds in surface water using solid-phase extraction

Wenfeng SUN, Ruibao JIA, Baoyu GAO

《环境科学与工程前沿（英文）》 2012年 第6卷 第1期   页码 66-74 doi: 10.1007/s11783-010-0257-3

摘要： In this paper, a method using solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) was developed to simultaneously analyze five taste and odor compounds in surface water, i.e., 2-methylisoborneol (2-MIB), 2,4,6-trichloroanisole (TCA), 2-isopropyl-3-methoxy pyrazine (IPMP), 2-isobutyl-3-methoxy pyrazine (IBMP), and -1,10-dimethyl- -9-decalol (geosmin, GSM). The mass spectrometry was operated in selective ion monitoring (SIM) mode. Three kinds of SPE columns and three eluting solvents were compared, the C18 column was chosen as optimum SPE column, and methanol was chosen as the optimum eluting solvent. It was found that the method showed good linearity in the range of 1–200 ng·L and gave detection limits of 0.5–1.5 ng·L for individual compounds. Good recoveries (93.5%–108%) and relative standard deviations (1.58%–7.31%) were also obtained. Additionally, concentrations of these taste and odor compounds in Jinan’s surface and drinking water were analyzed by applying this method, and the results showed that GSM and 2-MIB were the dominant taste and odor compounds in Jinan’s raw water.

关键词： solid-phase extraction (SPE)     gas chromatography-mass spectrometry (GC-MS)     taste and odor compounds     surface water     micropollutant    

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An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal

Feng Zhu, Zhijian Yao, Wenliang Ji, Deye Liu, Hao Zhang, Aimin Li, Zongli Huo, Qing Zhou

《环境科学与工程前沿（英文）》 2020年 第14卷 第3期 doi: 10.1007/s11783-020-1228-y

摘要： A hydrophilic resin (GCHM) was facile synthesis and characterized. Average absolute recovery of GCHM (75.6%) performs better than Oasis® HLB. Detection limits of method (SPE-UPLC-MS/MS) ranged between 0.03 and 0.6 ng/L. 22 PPCPs were determined in environmental waters ranging from 0.5 to 1590 ng/L. In this study, a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-co-divinylbenzene), characterized, and applied as a solid-phase extraction (SPE) material. Up to 44 pharmaceuticals and personal care products (PPCPs) belonging to 10 classes were recovered in environmental water samples. Different variables affecting extraction, such as adsorbent amount, sample pH, and loading speed, were optimized. Under optimal conditions, the average absolute recovery of 44 PPCPs was 75.6% using GCHM, indicating a better performance than the commercial Oasis® HLB. SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated, and the method achieved good linearity (r2>0.991, for all analytes). In addition, the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L. The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River, Huaihe River, and Taihu Lake, 1 groundwater sample from Changzhou in Jiangsu Province, 1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province, China. In these samples, 22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.

关键词： Hydrophilic resin     Solid phase extraction     Pharmaceuticals and personal care product     Ultra-performance liquid chromatography and tandem mass spectrometry     Environmental water    

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Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

Xueqi Fan, Jie Gao, Wenchao Li, Jun Huang, Gang Yu

《环境科学与工程前沿（英文）》 2020年 第14卷 第1期 doi: 10.1007/s11783-019-1187-3

摘要： • Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.

关键词： Pharmaceuticals and personal care products (PPCPs)     Isotopically labeled standard (ILSs)     Water     Solid-phase extraction (SPE)     LC-MS/MS    

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A magnetic adsorbent based on salicylic acid-immobilized magnetite nano-particles for pre-concentration of Cd(II) ions

Hossein Abdolmohammad-Zadeh, Arezu Salimi

《化学科学与工程前沿（英文）》 2021年 第15卷 第2期   页码 450-459 doi: 10.1007/s11705-020-1930-0

摘要： In this research, an eco-friendly magnetic adsorbent based on Fe O /salicylic acid nanocomposite was fabricated using a facile one-pot co-precipitation method. The crystalline and morphological characterization of the prepared nanocomposite was performed by field emission scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. The nanocomposite was employed as a magnetic solid-phase extraction agent for separation of Cd(II) ions from synthetic solutions. Some experimental factors affecting the extraction efficiency were investigated and optimized. Following elution with acetic acid (pH 3.5), the pre-concentrated analyte was quantified by flame atomic absorption spectrometry. In optimal conditions, a linear calibration graph was achieved in the concentration range of 0.2‒30 ng·mL with a determination coefficient ( ) of 0.9953. The detection limit, the enhancement factor, inter- and intra-day relative standard deviations (for six consecutive extractions at the concentration level of 10 ng·mL ) were 0.04 ng·mL , 100, 2.38% and 1.52%, respectively. To evaluate the accuracy of the method, a certified reference material (NIST SRM 1643e) was analyzed, and there was a good agreement between the certified and the measured values. It was successfully utilized to determine cadmium in industrial wastewater samples and the attained relative recovery values were between 96.8% and 103.2%.

关键词： cadmium     magnetic solid-phase extraction     Fe3O4 nanoparticles     Fe3O4/salicylic acid nanocomposite     flame atomic absorption spectrometry    

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Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum(LLE-GCMS) and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

MA Xiaoyan, CHEN Beibei, LI Qingsong, ZHANG Qiaoli, GU Guofen

《环境科学与工程前沿（英文）》 2007年 第1卷 第3期   页码 286-291 doi: 10.1007/s11783-007-0048-7

摘要： Two sample preparation methods were introduced and compared in this paper to establish a simple, quick and exact analysis of geosmin and 2-methylisoborneol. LC-18 column was employed in solid phase extraction (SPE), 1.0 mL of hexane was adopted in liquid-liquid extraction (LLE), and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode. Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB) and geosmin (GSM) with values below 50%. For LLE, the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM. Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB. A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer, there was a serious odor problem induced by a high concentration of 2-MIB. The highest concentration of 152.82 ng/L appeared in July in raw water, while GSM flocculation was minimal with concentrations below odor threshold.

关键词： summer     flocculation     simple     Shanghai     spectrum    

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Highly effective extraction of oil from soybean by pretreatment of solid-state fermentation with fungi

Xiaojuan NIU, Shuyi QIU, Yuangen WU, Jie YUAN, Yingying XU

《化学科学与工程前沿（英文）》 2011年 第5卷 第1期   页码 122-125 doi: 10.1007/s11705-010-0533-6

摘要： The solid-state prefermentation by (CICC 2377) and (CICC 40536) was employed to increase the oil extraction yield from soybean. The influence of incubation time on oil yield was investigated. The maximum oil yield extracted from the substrate prefermented by for 96 h was 23%, which increased by 47.4% compared with control (15.6%). In the same fermentation conditions, the maximum oil yield extracted from substrate prefermented by was 21.6%, which increased by 38.5% compared with control (15.6%). The quality of soybean oil was not changed obviously by the pretreatment of fermentation with fungi.

关键词： soybean     Aspergillus niger     Aspergillus flavus     solid-state fermentation     extraction of oil    

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Fully automatic container terminals of Shanghai Yangshan Port phase IV

Jack Xunjie LUO

《工程管理前沿（英文）》 2019年 第6卷 第3期   页码 457-462 doi: 10.1007/s42524-019-0053-0

摘要：

Engineering Owner: Construction Headquarters of Yangshan Deep-water Port Phase IV Project of Shanghai International Shipping Center

关键词： Yangshan Port     automated equipment     intelligent system     container terminals     port engineering    

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Phase transition regulation and caloric effect

《能源前沿（英文）》 2023年 第17卷 第4期   页码 463-477 doi: 10.1007/s11708-023-0860-1

摘要： Solid state refrigeration based on caloric effect is regarded as a potential candidate for replacing vapor-compression refrigeration. Numerous methods have been proposed to optimize the refrigeration properties of caloric materials, of which single field tuning as a relatively simple way has been systemically studied. However, single field tuning with few tunable parameters usually obtains an excellent performance in one specific aspect at the cost of worsening the performance in other aspects, like attaining a large caloric effect with narrowing the transition temperature range and introducing hysteresis. Because of the shortcomings of the caloric effect driven by a single field, multifield tuning on multicaloric materials that have a coupling between different ferro-orders came into view. This review mainly focuses on recent studies that apply this method to improve the cooling performance of materials, consisting of enlarging caloric effects, reducing hysteresis losses, adjusting transition temperatures, and widening transition temperature spans, which indicate that further progress can be made in the application of this method. Furthermore, research on the sign of lattice and spin contributions to the magnetocaloric effect found new phonon evolution mechanisms, calling for more attention on multicaloric effects. Other progress including improving cyclability of FeRh alloys by introducing second phases and realizing a large reversible barocaloric effect by hybridizing carbon chains and inorganic groups is described in brief.

关键词： phase transition regulation     caloric effect     solid state refrigeration    

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Combination of steam-enhanced extraction and electrical resistance heating for efficient remediation

《环境科学与工程前沿（英文）》 2022年 第16卷 第11期 doi: 10.1007/s11783-022-1582-z

摘要：

● Coupling merits of SEE and ERH were explored by a laboratory-scale device.

关键词： Steam-enhanced extraction     Electrical resistance heating     Dense nonaqueous phase liquid     Soil remediation     Energy consumption    

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Ultrafast solid-liquid-vapor phase change of a thin gold film irradiated by femtosecond laser pulses

Jing HUANG, Yuwen ZHANG, J. K. CHEN, Mo YANG

《能源前沿（英文）》 2012年 第6卷 第1期   页码 1-11 doi: 10.1007/s11708-012-0179-9

摘要： Effects of different parameters on the melting, vaporization and resolidification processes of thin gold film irradiated by femtosecond pulses and pulse train were systematically studied. The classical two-temperature model was adopted to depict the non-equilibrium heat transfer in electrons and lattice. The melting and resolidification processes, which was characterized by the solid-liquid interfacial velocity, as well as elevated melting temperature and depressed solidification temperature, was obtained by considering the interfacial energy balance and nucleation dynamics. Vaporization process which leads to ablation was described by tracking the location of liquid-vapor interface with an iterative procedure based on energy balance and gas kinetics law. The parameters in discussion included film thickness, laser fluence, pulse duration, pulse number, repetition rate, pulse train number, etc. Their effects on the maximum lattice temperature, melting depth and ablation depth were discussed based on the simulation results.

关键词： melting     evaporation     nucleation dynamics     nanoscale heat transfer    

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Coupled solid-fluid FE-analysis of an embankment dam

Michael PERTL, Matthias HOFMANN, Guenter HOFSTETTER

《结构与土木工程前沿（英文）》 2011年 第5卷 第1期   页码 53-62 doi: 10.1007/s11709-010-0084-4

摘要： A coupled solid-fluid FE-model for partially saturated soils, characterized by modeling the soil as a three-phase material consisting of a deformable soil skeleton and the fluid phases water and air, is reviewed briefly. As a constitutive model for the soil skeleton, the well-known Barcelona Basic model (BBM) is employed, which is formulated in terms of net stress and matric suction. For the BBM, a computationally efficient return mapping algorithm is proposed, which only requires the solution of a scalar nonlinear equation at the integration point level. The coupled FE-model is applied to the coupled transient numerical simulation of the water flow and the deformations and stresses in an embankment dam.

关键词： multi-phase model     unsaturated soil model     Barcelona Basic model (BBM)     return mapping algorithm     embankment dam    

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基于判别扩散映射分析的内蕴特征提取方法在刀具磨损评估中的应用 None

Yi-xiang HUANG, Xiao LIU, Cheng-liang LIU, Yan-ming LI

《信息与电子工程前沿（英文）》 2018年 第19卷 第11期   页码 1352-1361 doi: 10.1631/FITEE.1601512

摘要： 针对铣削加工刀具磨损评估，提出一种基于判别扩散映射分析的方法。判别扩散映射分析（discriminant diffusion maps analysis，DDMA）用于时频域特征提取融合与维度缩减。通过保持内蕴特征空间的扩散距离，耦合时频域特征和判别内核，提取有效信息。该方法包含3个步骤：(1)信号处理与特征提取；(2)内蕴维度估计；(3)基于扩散距离保持的特征融合实现。将该方法应用于数控加工中心主轴驱动电流信号，评估刀具磨损状态。与常见主成分分析方法相比，该方法能更好保持刀具磨损状态相关的有用内蕴信息，大大降低与刀具磨损相关的特征维度，并可直接应用于大多数工业数控加工中心，方便获取电流信号实际情况。

关键词： 刀具状态监测；流形学习；降维；扩散映射分析；内蕴特征提取    

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标题 作者 时间 类型 操作

Determination of selected semi-volatile organic compounds in water using automated online solid-phaseextraction with large-volume injection/gas chromatography/mass spectrometry

Yongtao LI, Christina L. MCCARTY, Ed J. GEORGE

期刊论文

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

Yunling Gao,Ying Hu,Kejian Yao

期刊论文

aniline derivatives in water samples after preconcentration with oxidized multiwalled carbon nanotubes as solid-phaseextraction disk

Hideyuki KATSUMATA, Yuta ODA, Satoshi KANECO, Tohru SUZUKI, Kiyohisa OHTA

期刊论文

Simultaneous analysis of five taste and odor compounds in surface water using solid-phase extraction

Wenfeng SUN, Ruibao JIA, Baoyu GAO

期刊论文

An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal

Feng Zhu, Zhijian Yao, Wenliang Ji, Deye Liu, Hao Zhang, Aimin Li, Zongli Huo, Qing Zhou

期刊论文

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

Xueqi Fan, Jie Gao, Wenchao Li, Jun Huang, Gang Yu

期刊论文

A magnetic adsorbent based on salicylic acid-immobilized magnetite nano-particles for pre-concentration of Cd(II) ions

Hossein Abdolmohammad-Zadeh, Arezu Salimi

期刊论文

Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum(LLE-GCMS) and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

MA Xiaoyan, CHEN Beibei, LI Qingsong, ZHANG Qiaoli, GU Guofen

期刊论文

Highly effective extraction of oil from soybean by pretreatment of solid-state fermentation with fungi

Xiaojuan NIU, Shuyi QIU, Yuangen WU, Jie YUAN, Yingying XU

期刊论文

Fully automatic container terminals of Shanghai Yangshan Port phase IV

Jack Xunjie LUO

期刊论文

Phase transition regulation and caloric effect

期刊论文

Combination of steam-enhanced extraction and electrical resistance heating for efficient remediation

期刊论文

Ultrafast solid-liquid-vapor phase change of a thin gold film irradiated by femtosecond laser pulses

Jing HUANG, Yuwen ZHANG, J. K. CHEN, Mo YANG

期刊论文

Coupled solid-fluid FE-analysis of an embankment dam

Michael PERTL, Matthias HOFMANN, Guenter HOFSTETTER

期刊论文

基于判别扩散映射分析的内蕴特征提取方法在刀具磨损评估中的应用

Yi-xiang HUANG, Xiao LIU, Cheng-liang LIU, Yan-ming LI

期刊论文