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JOURNAL OF CHROMATOGRAPHY A · 2016 · IF 3.926

Carbon nanotube composite microspheres as a highly efficient solid-phase microextraction coating for sensitive determination of phthalate acid esters in water samples

Xin-Li Song,Yue Chen,Jin-Peng Yuan,Yu-Jun Qin,Ru-Song Zhao,Xiao Wang

Multiwalled carbon nanotubes (MWCNTs) on polystyrene (PS) microspheres have been designed and prepared by layer-by-layer assembly via electrostatic interaction. MWCNTs@PS was characterized by scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The new materials were employed as a novel solid-phase microextraction (SPME) coating to enrich trace level of phthalate acid esters (PAEs) in water samples. Five PAEs, di- n -butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexyl adipate (DEHA), di-2-ethylhexyl phthalate (DEHP) and di- n -octyl phthalate (DOP), were studied in this work. The Box-Behnken design was applied to calculate optimum extraction factors affecting the extraction efficiency using a response surface. In the optimized conditions, the developed technique achieved high enrichment factors (738–2347), low limits of detection (0.0012–0.018   μg   L −1 ) and wide linearity (0.001–5   μg   L −1 ) for detecting PAEs. The method was successfully applied to analyze PAEs in real environmental water samples with recovery ranging from 73.4% to 103.8%. The results demonstrated that MWCNTs@PS are a promising coating material in the SPME of PAEs at trace levels from environmental samples.

研究领域: 环境科学 · 分析化学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2018 ·Vol. 411 ·期 2 ·507-515 · IF 3.307

Carboxyl Fe3O4 magnetic nanoparticle-based SPE and HPLC method for the determination of six tetracyclines in water

Yang Yi,Yin Shuo,Yang Danni,Jiang Yang,Li Yongxin,Zhou Chen,Sun Chengjun

A novel carboxyl Fe 3 O 4 magnetic nanoparticle-based solid-phase extraction combined with high-performance liquid chromatography was developed for the analysis of oxytetracycline, tetracycline, demeclocycline, metacycline, chlortetracycline, and doxycycline in water samples. Driven by the electrostatic interaction and the strong chelation between tetracyclines and iron ions, tetracyclines in samples were adsorbed onto the adsorbents. The adsorbed analytes were subsequently eluted with oxalic acid and separated with a C 18 column under gradient condition with a mobile phase consisting of methanol, acetonitrile, and oxalic acid at a flow rate of 0.5 mL/min. The detection was performed at variable ultraviolet wavelengths. Under optimized conditions, the developed method gave an enrichment factor of 33.3, linearity ranges of 5.00–1000 μg/L, detection limits of (2.86–5.19) × 10 -2 μg/L, quantification limits of (9.54–17.3) × 10 -2 μg/L, recoveries of 76.2–98.0%, and intra- and inter-day RSDs of 0.132–15.5% and 2.28–14.5% for these tetracyclines. The established method was successfully applied for the determination of these six tetracyclines in tap water, river water, pond water, and lake water samples. ᅟ

研究领域: 环境科学 · 分析化学
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JOURNAL OF FLUORESCENCE · 2017 ·Vol. 27 ·期 4 ·1421-1426 · IF 1.461

Fluorescence Detection of p-Nitrophenol in Water Using Bovine Serum Albumin Capped ag Nanoclusters

Mao Mi,Deng Chun,He Yu,Ge Yili,Song Gongwu

We developed a sensitive and selective method for detection of 4-Nitrophenol (PNP) using Ag nanoclusters (NCs) as fluorescence probe. Bovine serum albumin (BSA) was used as the template for preparing Ag NCs via wet chemistry. The fluorescence of as-prepared Ag NCs was significantly quenched in the presence of PNP, showing excellent linear relationships between the quenching degree of the fluorescence intensity and the concentrations of PNP in the range of 0.5 μM to 60 μM. The fluorescence quenching mechanism was also investigated. Furthermore, this method was applied for the recognition of PNP in environmental samples.

CAS / MDL: 9048-46-8 7761-88-8
研究领域: 分析化学 · 环境科学 · 生物医学
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MICROCHIMICA ACTA · 2017 ·Vol. 184 ·期 8 ·2981-2990 · IF 4.58

Magnetic solid phase extraction of non-steroidal anti-inflammatory drugs from water samples using a metal organic framework of type Fe3O4/MIL-101(Cr), and their quantitation by UPLC-MS/MS

Wang Ting,Liu Siyu,Gao Guihua,Zhao Pan,Lu Nan,Lun Xiaowen,Hou Xiaohong

The authors describe a method for magnetic solid phase extraction (MSPE) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the quantitation of eight non-steroidal anti-inflammatory drugs (NSAIDs) in wastewater and environmental water samples. Specifically, the NSAIDs were directly extracted by using a magnetic nanocomposite of type Fe 3 O 4 /MIL-101(Cr) (Matérial Institute Lavoisier, MIL) from 50 mL water samples without any further cleanup. The effects of the amount of adsorbent, pH value, salt concentration, ultrasonic extraction time, desorption solvent nature and volume and desorption time were investigated. Under the optimal conditions, UPLC-MS/MS based detection resulted in the following figures of merit: (a) Linear calibration plots that typically extend from 0.1 (0.2, 0.05, 0.02) to 50 μg·L −1 , depending on the compound; (b) detection limits between 3 to 60 ng·L −1 ; and (c), recoveries varying from 81.2% to 116.8% with relative standard deviations between 0.4% and 10.8%. The adsorption of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was characterized by adsorption isotherms, kinetics and thermodynamics studies and provides a deeper insight into the adsorption mechanism. Compared to other method for pretreatment and preconcentration of NSAIDs, the new method is more rapid, sensitive, accurate and eco-friendly. The method was successfully applied to the determination of the NSAID residues in a variety of real environmental and wastewater samples. Schematic of a method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in environmental water by magnetic solid phase extraction based on Fe 3 O 4 /MIL-101(Cr) combined with UPLC-MS/MS. The adsorption mechanism of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was studied.

CAS / MDL: 1317-61-9
研究领域: 环境科学 · 分析化学
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ELECTROPHORESIS · 2016 ·Vol. 37 ·期 19 ·2502-2508 · IF 2.482

Dispersive liquid-liquid microextraction for four phenolic environmental estrogens in water samples followed by determination using capillary electrophoresis

Junying Liu,Wenhui Lu,Huitao Liu,Xiaqing Wu,Jinhua Li,Lingxin Chen

Dispersive liquid-liquid microextraction (DLLME) coupled with CE was successfully developed for simultaneous determination of four types of phenolic environmental estrogens (PEEs), namely hexestrol (HS), bisphenol A (BPA), diethylstilbestrol (DES) and dienestrol (DS). Several parameters affecting DLLME and CE conditions were systematically investigated including the type and volume of extraction solvent and dispersive solvent, extraction time, salt, pH value, surfactant, buffer solution and so on. Under the optimal conditions, DLLME-CE exhibited strong enrichment ability, presenting high enrichment factors of 467, 241, 367 and 362 for HS, BPA, DES and DS, respectively, as well as low detection limits of 0.3, 0.6, 0.6 and 0.3 μg/L, respectively. Excellent linearity was achieved in the range of 2.0–150 μg/L for HS and DS, and 4.0–300 μg/L for BPA and DES, with correlation coefficients R >0.9983. Recoveries ranging from 70.4 to 108.1% were obtained with tap water, lake water and seawater samples spiked at three concentration levels and the relative standard deviations (RSDs, for n = 5) were 2.1–9.7%. This DLLME-CE method with high selectivity and sensitivity, high stability, simplicity, cost-effectiveness, eco-friendliness was proved potentially applicable for the rapid and simultaneous determination of PEEs in complicated water samples.

CAS / MDL: 56-23-5 151-21-3
研究领域: 分析化学 · 环境科学
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ANALYTICA CHIMICA ACTA · 2017 · IF 4.95

Low-cost and convenient ballpoint tip-protected liquid-phase microextraction for sensitive analysis of organic molecules in water samples

Baocheng Ji,Bing Xia,Xian Fu,Shan Lei,Ye Ye,Yan Zhou

Simplification and miniaturization in analytical procedures are highly preferred by analysts and other researchers. In this study, a low-cost, convenient and efficient liquid-phase microextraction method, termed ballpoint tip-protected liquid-phase microextraction (BT-LPME), was established. The bullet-shaped BT possessed a hollow cavity of several microliters for solvent storage and an opening tail for solute extraction. Magnetic field-induced BT spinning significantly accelerated the extraction process. By virtue of the adhesion between a stainless steel sheath and an organic solvent , along with cave protection, finely stable storage of extractant was achieved even under high spinning speeds (>1000 rpm). The BT-LPME performance was evaluated by extracting five polycyclic aromatic hydrocarbons (PAHs) from aqueous solution, followed by gas chromatography-mass spectrometry (GCMS) analysis. Compared to static single drop microextraction (SDME), the BT-LPME method provided higher enrichments (128–173-fold) for the five PAHs. Good linearities (from 0.01∼0.05 μg L −1 to 50 μg L −1 ) with a regression coefficient (r 2 ) ≥0.9993, as well as low limits of detection (LODs, 0.002–0.011 μg L −1 ) and limits of quantification (LOQs, 0.007–0.023 μg L −1 ), were obtained. Relative recoveries varied from 92.3% to 103.4% at three spiked levels of 0.1, 1 and 10 μg L −1 . The BT-LPME technique was also successfully applied to the enrichment of other organic compounds, such as organophosphorus compounds , organochlorines and triazines .

研究领域: 分析化学 · 环境科学
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OPTICAL MATERIALS · 2022 · IF 3.754

Enhanced ratiometric fluorescence molecularly imprinted nanosensor based on CDs for selective and visual detection of NOR in water samples

Tongfei Wu,Bo Hu,Jie Lv,Yunhui Li,Jing Shao,Yuqin Ma,Yuan Cui

Norfloxacin plays an indispensable part in the field of the medical industry, stock raising, and aquaculture. However, excessive use of NOR can induce serious harmful effects on humans and antibiotic resistance of organisms. In this work, a novel fluorescence-enhanced ratiometric fluorescence imprinted sensor was constructed and used to realize selective and accurate detection of NOR. CdTe quantum dots encapsulated in silicon dioxide acted as the reference signal and CDs doped in the imprinted layer as the response signal. Under optimal conditions, NOR rapidly enhanced the fluorescence of CdTe@SiO 2 @FMIPs at 435 nm with 1 min and exhibited excellent linear relationships between the fluorescence enhancement efficiency and the NOR concentration over 10–90 nM with a detection limit of 3.28 nM. Due to the interaction of NOR and CDs through hydrogen bonding as well as π-π conjugation, the visual detection for NOR was achieved by distinguishing the color change from red to bright blue. Satisfied recovery rates of 93.4%–107.7% and RSD of 2.0%–3.6% were gained by actual sample experiments. Furthermore, CdTe@SiO 2 @FMIPs made it possible to reuse at least 5 times.

研究领域: 环境科学 · 分析化学
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

A new sample treatment strategy based on supramolecular solvent for determination of herbicide residues in water samples by Box-Behnken design

Ruiyu Fu,Tingze Ren,Yanhui Zhang,Xiaoli Guo,Xin Di

This paper describes a sensitive, simple and green analytical method for pretreatment of sulfonylurea and pyrethroid herbicides in water samples by supramolecular solvent-based liquid phase microextraction (SUPRAS-LPME). The SUPRAS was rapidly formed by nonanoic acid and tetrahydrofuran (THF)/water solution. The attractive features of SUPRAS-LPME include the simplicity, high enrichment factor, low cost and less consumption of organic solvents. The main influencing factors including type and volume of fatty acids, volume of THF , ionic strength, vortex time and volume of formic acid were optimized in detail, and then the significant variables were optimized by Box-Behnken design (BBD). Under the optimized condition, the proposed method shows high precision (RSDs  <  13.7 %), low limits of detection (0.5–10 μg L -1 ) and limits of quantitation (10–45 μg L -1 ), acceptable recovery (71.3 %-95.9 %). The proposed method was successfully applied for analysis of sulfonylurea and pyrethroid herbicides in water samples, making it an alternative analytical strategy for determination of trace analytes at the microgram per liter range with desirable sensitivity.

研究领域: 分析化学 · 环境科学
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Room-temperature synthesis of ionic liquid@covalent organic frameworks for the solid phase extraction and analysis of six herbicides from water samples

Liling Wang,Yanbin Wang,Yuchuan Qin,Yifeng Zhou

Waters contaminated with pesticides poses a potential hazard to ecosystems and human health, so sensitive and efficient analytical methods are essential for water monitoring. Herein, in order to efficiently extract six commonly used herbicides, a novel ionic liquid covalent organic framework (IL@COF) was prepared using a simple room-temperature synthesis in this study. As an adsorbent for solid phase extraction (SPE), the mesoporous material exhibits rapid adsorption performance for six typical herbicides from water samples. Under the optimal experimental conditions, wide linearities (500 ∼ 20,000 μg L –1 ) and low limits of detection (prometryn: 17.9 μg L –1 ; metribuzin: 36.7 μg L –1 ; bentazon: 14.5 μg L –1 ; isoproturon: 18.0 μg L –1 ; acetochlor: 19.6 μg L –1 ; butachlor: 37.1 μg L –1 ) for six analytes were obtained via high performance liquid chromatography (HPLC). The adsorbent has stable physical and chemical properties and can be reused for 10 times after effective elution. The applicability of this method is further evaluated by analyzing ten kinds of real water sample. The recoveries of six kinds of herbicides ranged from 85.3 % to 122.9 %. The mechanism of adsorption is the interaction between hydrogen bond acceptor and donor. These results indicate that HPLC after SPE with a new type of IL@COF as the SPE adsorbent is a promising technique for the simultaneous detection of six pesticides in environmental water samples.

研究领域: 环境科学 · 分析化学
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Analytical Methods · 2019 ·Vol. 11 ·期 40 ·5214-5221 · IF 2.378

Synthesis of nitrogen and sulfur codoped carbon dots and application for fluorescence detection of Cd(II) in real water samples

Mingyu Tang,Xiaodong Liu,Nannan Zhang,Jingyu Pang,Yu Zou,Fang Chai,Hongbo Wu,Lihua Chen

Herein, nitrogen and sulfur codoped carbon dots (N&S CDs) were prepared by a facile hydrothermal process and they could be introduced as a fluorescent probe for the determination of cadmium ions (Cd2+), yielding high sensitivity and excellent selectivity. The obtained N&S CDs exhibited bright blue fluorescence with a quantum yield of 40% and exhibited a fast responsive fluorescence quenching signal within 2 min toward Cd2+ in both ultrapure water and real water samples. The CDs responded to Cd2+, which acted as a quencher of blue fluorescence at 459 nm with the limit of detection of 0.018 μM in the range of 0.02–1 μM. The quenching fluorescence behavior was found to obey the static quenching effect (SQE). The low toxicity and good cell permeability of CDs were verified by cell experiments.

研究领域: 分析化学 · 环境科学 · 纳米材料 · 生物传感 · 环境污染监测
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Methods and Applications in Fluorescence · 2017 ·Vol. 5 ·期 1 ·015003 · IF 2.656

One-pot carbonization synthesis of europium-doped carbon quantum dots for highly selective detection of tetracycline

Meng Li Liu,Bin Bin Chen,Tong Yang,Jian Wang,Xi Dong Liu,Cheng Zhi Huang

The detection of tetracycline is of great significance because of its damaging effects on human health, such as renal toxicity and hemolytic anemia. Any release of tetracycline into the surrounding environment can produce bacterial drug resistance. We develop a new sensitive and selective detection approach for tetracycline in complex water samples by preparing europium-doped carbon quantum dots (Eu-CQDs) through a simple and rapid carbonization method operating at 200 °C for 5 min. The Eu-CQDs are characterized by blue photoluminescence, excitation-wavelength-dependent emission and excellent stability. Importantly, the fluorescence of the Eu-CQDs can be quenched efficiently by tetracycline, based on the strong inner filter effect mechanism between Eu-CQDs and tetracycline, making the fluorescence intensity ratio (I0/I) of the Eu-CQDs at 465 nm correlate linearly with the concentration of tetracycline in the range of 0.5–200 μM, with a limit of detection of 0.3 μM. This shows the broad applicability of the Eu-CQDs in pursuing the concepts of simplicity and specificity for analytical purposes.

研究领域: 分析化学 · 环境科学 · 生物医学
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JOURNAL OF CHROMATOGRAPHY A · 2017 · IF 3.981

Extraction of trace polychlorinated biphenyls in environmental waters by well-dispersed velvet-like magnetic carbon nitride nanocomposites

Dandan Li,Jun Zhu,Man Wang,Wentao Bi,Xiaohua Huang,David Da Yong Chen

A velvet-like magnetic carbon nitride nanocomposites synthesized by chemical co-precipitation was used to develop a highly efficient magnetic solid-phase extraction method for the pre-concentration of trace polychlorinated biphenyls (PCBs) in water samples. The advantages of this nanocomposite such as large surface area, good dispersity, low solvent consumption, rapid analyte adsorption (30   s) and reusability make it a good sorbent. Factors affecting extraction efficiency were systematically investigated and optimized by response surface methodology (RSM). Under optimal experimental conditions, the limits of detection (LODs S/N   =   3) of the developed method for PCBs investigated were in the range of 9.0   ×   10 −6 –5.8   ×   10 −5   μg/mL. This method was then used for the analysis of four real water samples. Good spiked recoveries over the range of 80.1-118.4%, and RSDs (n   =   5) of 0.02–3.7% were obtained. This work demonstrated the potential of using this nanocomposite for adsorption, pre-concentration, or even removal of different carbon-based aromatic compounds or other hydrophobic pollutants.

研究领域: 环境科学 · 分析化学
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