JOURNAL OF CHROMATOGRAPHY A
·
2013
·
IF 4.612
Xingmei Guan,Chuande Zhao,Xiaoyan Liu,Haixia Zhang
A polymer monolith column was prepared using click chemistry for on-line solid phase microextraction of polycyclic aromatic hydrocarbons (PAHs), using 2,2′,7,7′-tetraethynyl-9,9′-spirobifluorene(TES) and 1,4-bis(6-azidoalkoxy)benzene (BAB) as monomers, and Cu(PPh 3 ) 3 Br as the catalyst. The polymer with spirocyclic cross-links was porous and presented an appropriate interspace of PAHs. Enrichment of PAHs, in the range of 100 to more than 1000 times, was due to the π – π stacking interaction and the effect of small size. The factors affecting the on-line microextraction efficiency were optimized, and the analytical conditions were evaluated to ensure reliability.
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高影响因子
Environmental Science-Processes & Impacts
·
2014
·Vol. 17
·期 2
·488-494
·
IF 0
Xiaozhu Wei,Ping Gu,Guanghui Zhang,Jianjun Huang
This paper aimed to investigate the occurrence and concentrations of emerging and priority pollutants in the municipal reverse osmosis concentrate (ROC) using liquid–liquid extraction (LLE) followed by gas chromatography-mass spectrometry. The results indicated that there were varieties of pollutants, including chlorinated organic compounds, polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PAEs), pharmaceutical and personal care products (PPCPs), herbicides and flame retardants, in the ROC. Most of the pollutants were quantified, and the performance of the analytical method was explored. For most of the target compounds, the mean recoveries at two concentration levels (0.17 μg L−1 and 1.67 μg L−1) ranged from 70% to 130% and the relative standard deviation (RSD) values were less than 20%, indicating excellent accuracy and precision. Typical concentrations of most of the pollutants were as low as tens or hundreds of ng L−1, whereas others were as high as several μg L−1 (such as, the concentration of 2-chloroethyl ether was 1.42 μg L−1, of caffeine was 3.73 μg L−1, and of benzyl butyl phthalate was 4.90 μg L−1).
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TALANTA
·
2014
·
IF 3.511
Guijiang Zhang,Xiaohuan Zang,Zhi Li,Chun Wang,Zhi Wang
In this study, polydimethylsiloxane/metal-organic frameworks (PDMS/MOFs), including PDMS/MIL-101 and PDMS/MOF-199, were immobilized onto a stainless steel wire through sol–gel technique as solid-phase microextraction (SPME) fiber coating. The prepared fibers were used for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatography–mass spectrometry (GC–MS) analysis. Under the optimized experiment conditions, the PDMS/MIL-101 coated fiber exhibited higher extraction efficiency towards PAHs than that of PDMS/MOF-199. Several parameters affecting the extraction of PAHs by SPME with PDMS/MIL-101 fiber, including the extraction temperature, extraction time, sample volume, salt addition and desorption conditions, were investigated. The limits of detection (LODs) were less than 4.0 ng L −1 and the linearity was observed in the range from 0.01 to 2.0 µg L −1 with the correlation coefficients ( r ) ranging from 0.9940 to 0.9986. The recoveries of the method for the PAHs from water samples at spiking levels of 0.05 and 0.2 µg L −1 ranged from 78.2% to 110.3%. Single fiber repeatability and fiber-to-fiber reproducibility were less than 9.3% and 13.8%, respectively.
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JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Xingru Hu,Chao Liu,Jiansheng Li,Rui Luo,Hui Jiang,Xiuyun Sun,Jinyou Shen,Weiqing Han,Lianjun Wang
In this study, a novel hollow mesoporous carbon spheres-based fiber (HMCSs-F) was fabricated to immobilize HMCSs onto a stainless steel wire for solid-phase microextraction (SPME). Characterization results showed that the HMCSs-F possessed a large specific surface area, high porosity and uniform pore size. To demonstrate the extraction performance, a series of polycyclic aromatic hydrocarbons (PAHs) was chosen as target analytes. The experimental parameters including extraction and desorption conditions were optimized. Compared to commercial fibers, the HMCSs-F exhibited better extraction efficiency for PAHs. More interestingly, a good extraction selectivity for PAHs from the complex matrix was observed in these HMCSs-F. The enhanced SPME performance was attributed to the unique pore structure and special surface properties of the HMCSs. Furthermore, under the optimum conditions, the limits of detection (LODs) for the HMCSs-F were in the range of 0.20–1.15 ng L −1 with a corresponding relative standard deviation that was below 8.6%. The method was successfully applied for the analysis of PAHs in actual environmental water samples with recoveries ranging from 85.9% to 112.2%. These results imply that the novel HMCSs-F have potential application in environmental water analysis.
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TALANTA
·
2017
·
IF 4.162
Yanzhe Li,Zhe Sheng,Chuanlei Zhu,Wei Yin,Changhu Chu
Crown ether is a type of typical macrocyclic polyether compounds, which can produce strong interactions with cationic species, such as metal ions and protonated amines due to its cavity structure and the strong electronegative effect of heteroatoms on the crown ether ring. In this paper, a type of silica based crown ether stationary phase was prepared by covalently bonding dibenzo-18-crown 6-ether (DBCE) on silica gel via copper (I) catalyzed azide-alkyne 1,3-dipolar cycloaddition (CuAAC). The tetraazido DBCE was rapidly prepared by bromomethylation and subsequent azido substitution of DBCE. Finally, this key intermediate was covalently bonded to silica beads by click chemistry to get click-DBCE. Its structure was confirmed by FT-IR and elemental analysis, and the structures of all related intermediates were confirmed by NMR, IR and MS spectra. The crown ether based stationary phase showed good chromatography characteristics and column efficiency (up to 43,553 plates m -1 theoretical plate number is obtained in the case of fluoranthene) under reverse phase liquid chromatographic (RPLC) model. The primary chromatographic evaluation showed that click-DBCE displayed better chromatography efficiency than commercial C18 stationary phase (THERMO BDS HYPERSIL), when they were applied in the separation of regio-isomers of benzene, polycyclic aromatic hydrocarbons (PAHs) and macrolide pharmaceuticals. Furthermore, this stationary phase could also be used to separate fullerenes under normal phase mode, and in this case, 1-chloronaphthalene was suitable additive for improving chromatographic separation ability.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Xiaohong Yang,Changxia Li,Meiling Qi,Liangti Qu
This work presents the separation performance of graphene-ZIF8 (G-Z) composite material as stationary phase for capillary gas chromatography (GC). The G-Z stationary phase achieved high column efficiency of 5000 plates/m determined by n -dodecane ( k = 1.22) at 120 °C and showed weakly polar nature. Importantly, it exhibited high selectivity and resolving capability for branched alkane isomers and aromatic positional isomers, showing clear advantages over the reported neat graphene and ZIF8. In addition, it attained high resolution for geometric cis -/ trans -isomers. The G-Z column exhibited good column thermal stability up to 300 °C and column repeatability with RSD values of retention times in the range of 0.01–0.19% for intra-day, 0.05–0.88% for inter-day and 0.66–5.6% for between-column, respectively, Moreover, the G-Z column was employed for the determination of minor impurity isomers in real reagent samples, which demonstrates its promising potential in GC applications .
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高影响因子
OPTICS EXPRESS
·
2016
·Vol. 24
·期 14
·A1148
·
IF 3.148
Ruifang Yang,Nanjing Zhao,Xue Xiao,Gaofang Yin,Shaohui Yu,Jianguo Liu,Wenqing Liu
It is still difficult to determine the concentrations of polycyclic aromatic hydrocarbons accurately in natural water by fluorescence technique because of their low solubility, different fluorescent intensity, and the complex interferents from water environments. In this work, three-way fluorescence spectra combined with three methods including three-way parallel factor analysis, multi-way partial least square with residual bilinearization and unfolded partial least square with residual bilinearization were used to predict the concentrations of polycyclic aromatic hydrocarbons at the μg L−1 level in reservoir and river water, respectively. The prediction abilities of these methods on different analytes were evaluated by validation sets. The results demonstrate that unfolded partial least square with residual bilinearization yields the optimal results with relative error less than or equal to 6% for phenanthrene, pyrene, anthracene and fluorene, and 35% for acenaphthene and fluoranthene in different water backgrounds.
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高影响因子
CHEMOSPHERE
·
2017
·
IF 4.208
Yong Li,Ling Long,Jing Ge,Li-xuan Yang,Jin-jin Cheng,Ling-xiang Sun,Changying Lu,Xiang-yang Yu
Polycyclic aromatic hydrocarbons (PAHs) accumulated in agricultural soils are likely to threaten human health and ecosystem though the food chain, therefore, it is worth to pay more attention to soil contamination by PAHs. In this study, the presence, distribution and risk assessment of 16 priority PAHs in rice-wheat continuous cropping soils close to industrial parks of Suzhou were firstly investigated. The concentrations of the total PAHs ranged from 125.99 ng/g to 796.65 ng/g with an average of 352.94 ng/g. Phenanthrene (PHE), fluoranthene (FLT), benzo [a] anthracene (BaA) and pyrene (PYR) were the major PAHs in those soil samples. The highest level of PAHs was detected in the soils around Chemical plant and Steelworks, followed by Printed wire board, Electroplate Factory and Paper mill. The composition of PAHs in the soils around Chemical plant was dominated by 3-ring PAHs, however, the predominant compounds were 4, 5-ring PAHs in the soils around other four factories. Meanwhile, the concentration of the total PAHs in the soils close to the factories showed a higher level of PAHs in November (during rice harvest) than that in June (during wheat harvest). Different with other rings of PAHs, 3-ring PAHs in the soils around Chemical plant and Steelworks had a higher concentration in June. The results of principal component analysis and isomeric ratio analysis suggested that PAHs in the studied areas mainly originated from biomass, coal and petroleum combustion. The risk assessment indicated that higher carcinogenic risk was found in those sites closer to the industrial park.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Yunzhong Zheng,Meiling Qi,Ruonong Fu
This work presents the first example of utilization of graphitic carbon nitride (g-C 3 N 4 ) as stationary phase for capillary gas chromatographic (GC) separations. The statically coated g-C 3 N 4 column showed the column efficiencies of 3760 plates/m and weak polarity. Its resolving capability and retention behaviours were investigated by using the Grob test mixture, and mixtures of diverse types of analytes, and structural and positional isomers. The results showed superior separation performance of the g-C 3 N 4 stationary phase for some critical analytes and preferential retention for aromatic analytes. Specifically, it exhibited high-resolution capability for aromatic and aliphatic isomers such as methylnaphthalenes and dimethylnaphthalenes , phenanthrene and anthracene and alkane isomers. In addition, g-C 3 N 4 column showed excellent thermal stability up to 280 °C and good repeatability with relative standard deviation (RSD) values less than 0.09% for intra-day, below 0.23% for inter-day and in the range of 1.9–8.4% for between-column, respectively. The advantageous separation performance shows the potential of g-C 3 N 4 and related materials as stationary phase in GC and other separation technologies.
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JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Shengju Liu,Jiaxi Peng,Hongyan Zhang,Xin Li,Zheyi Liu,Xiaohui Kang,Minghuo Wu,Ren’an Wu
An organic-silica hybrid monolithic capillary column was fabricated by crosslinking (3-aminopropyl)trimethoxysilane (APTMS) modified mesoporous carbon nanoparticles (AP-MCNs) with tetramethoxysilane (TMOS) and n-butyltrimethoxysilane (C4-TriMOS). Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy, mercury intrusion porosimetry and inverse size-exclusion chromatography characterization proved the successful immobilization of mesoporous carbon nanoparticles (MCNs). The crosslinking of AP-MCNs into the hybrid monolithic matrix has significantly increased the reversed-phase retention of alkylbenzenes and chromatographic performance for small molecules separations in comparison with the neat one without MCNs. The resulting column efficiency of the mesoporous carbon nanoparticle-based butyl-silica hybrid monolithic column (MCN-C4-monolith) was up to ca. 116,600 N/m for the capillary liquid chromatography (cLC) separation of butylbenzene. Enhanced performance of proteins separation was achieved on the MCN-C4-monolith in comparison with the butyl-silica hybrid monolithic column without MCN (C4-monolith). The separation of peptides from bovine serum albumin (BSA) digest was carried out on the MCN-C4-monolith by capillary liquid chromatography–tandem mass spectrometry (cLC–MS/MS) with protein sequence coverage of 81.9%, suggesting its potential application in proteomics.
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2017
·
IF 3.981
Yunzhong Zheng,Qing Han,Meiling Qi,Liangti Qu
Seaweed-like graphitic carbon nitride (g-C 3 N 4 ) has a unique porous architecture composed of interlocking g-C 3 N 4 nanofibers (NF-C 3 N 4 ) with much higher surface area than bulk g-C 3 N 4 and shows good potential in separation science. This work investigated the separation performance of NF-C 3 N 4 as stationary phase for capillary gas chromatographic (GC) separations. The NF-C 3 N 4 column exhibits weak polarity and high column efficiency of 4728 plates/m for n -dodecane. Importantly, it displays good separation performance for a wide range of analytes and shows different retention behaviors from the bulk g-C 3 N 4 column and commercial HP-5MS column with 5% phenylpolysiloxane. Particularly, it shows high resolving capability for both aliphatic and aromatic isomers. In addition, NF-C 3 N 4 column has high thermal stability up to 280 °C and good separation repeatability with relative standard deviation (RSD) values in the range of 0.29–0.61% for intra-day, 0.56–1.1% for inter-day and 2.0–4.9% for between-column, respectively. Moreover, it was applied for the determination of isomer impurities in real samples, showing good potential in GC applications.
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MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 7
·2171-2180
·
IF 4.58
Wu Tong,Wang Juntao,Liang Weiqian,Zang Xiaohuan,Wang Chun,Wu Qiuhua,Wang Zhi
The authors describe a three-dimensional single layer graphitic carbon nitride-modified graphene composite (g-C 3 N 4 @G) deposited on a stainless steel wire by a sol-gel technique. The coated fiber was applied to direct immersion solid-phase microextraction of trace levels of polycyclic aromatic hydrocarbons (PAHs) from cosmetics samples prior to their determination by gas chromatography with mass spectrometry (GC-MS). Due to π stacking interaction and hydrophobic interaction between the g-C 3 N 4 @G coating and the analytes (naphthalene, acenaphthene, fluorene, phenanthrene, fluoranthene and pyrene), the fiber displays an excellent adsorption capability for the analytes. Under optimized conditions, the method has a wide linear range, low LODs (from 1.0 to 2.0 ng L −1 ), good repeatability and high recoveries. It was successfully applied to the determination of PAHs in cosmetics. The g-C 3 N 4 @G fiber also exhibited good durability.
Schematic of a three-dimensional single layer graphitic carbon nitride-modified graphene composite (g-C 3 N 4 @G) that was coated onto a stainless steel wire for the direct-immersion solid phase microextraction of trace levels of polycyclic aromatic hydrocarbons prior to gas chromatography-mass spectrometric detection.
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