MICROCHIMICA ACTA
·
2014
·Vol. 182
·期 3
·737-744
·
IF 3.719
Yang Jing,Si Ling,Cui Shihai,Bi Wentao
We have developed a facile in-situ growth method for the deposition of magnetite (Fe 3 O 4 ) particles on the surface of a graphitic carbon nitride (g-C 3 N 4 ) nanosheet. The material was characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The high affinity of g-C 3 N 4 for phenolic acids in combination with the magnetism of Fe 3 O 4 provides an efficient means for magnetic solid phase extraction. The adsorption, desorption and recoveries were examined. Under optimized conditions, the method has limits of detection in the range from 17.5–42.6 ng mL −1 (at an S/N of 3), and precisions from 2.8–3.8 % (for n = 5). The method was successfully applied to the determination of protocatechuic, caffeic, and ferulic acids in Salicornia herbacea L . plant extracts. Recoveries ranged from 92.4–99.5 %.
The high affinity of g-C 3 N 4 toward the phenolic acids as well as the magnetic behavior of Fe 3 O 4 were combined in this nanocomposite material to provide an efficient and simple magnetic solid phase extraction (MSPE) approach.
研究领域:
材料科学
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分析化学
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环境科学
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产品关联
DOI
高影响因子
ANALYTICAL SCIENCES
·
2022
·Vol. 38
·期 1
·105-112
·
IF 1.967
Wu Xiaoxiao,Huang Jingjing,Zhang Chi,Kang Xuejun
A novel nanofiber-based solid phase extraction (NFSPE) coupled with HPLC–DAD was developed for the determination of salivary histidine, a new potential index of physiological events. The treatment of the sample was based on a coupling reaction of histidine with the diazotization products of sulfanilic acid and sodium nitrite in a slightly alkaline medium, followed by NFSPE. Nanofibers comprising polystyrene and zinc acetate were used as a novel solid-phase sorbent to extract derived histidine via the chelation of Zn 2+ with the imidazole group in the analyte. The eluted target compound was analyzed by HPLC–DAD. Good linearity was achieved with the concentrations of histidine ranging from 0.645 to 64.5 µM; the detection limit was 0.193 µM. The intra-day and inter-day coefficients of variation were less than 8.0%. The method was successfully applied to the determination of salivary histidine in the subjects exposed to a public speaking stress. Graphical abstract
研究领域:
分析化学
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生物医学
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材料科学
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产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Yu Wang,Qianzhan Yang,Huadong Zhang,Zhenghong Wang,Ailin Wu,Yun Luo,Qianru Zhou
Background The ongoing infusion of pharmaceutical and personal care products (PPCPs) into ecosystems sustains a perpetual life cycle and leads to multi-generational exposures. Limited understanding of their environmental impact and their intrinsic ability to induce physiological effect in humans, even at low doses, pose great risks to human health. Few scholarly works have conducted systematic research into the occurrence of PPCPs within potable water systems. Concurrently, the associated monitoring techniques have not been comprehensively examined with regards to the specific nature of drinking water, namely whether the significant presence of disinfectants may influence the detection of PPCPs. Results A modified approach in terms of detailed investigation of sample preservation and optimization of an in-lab fabricated solid phase extraction (SPE) cartridge filled with DVB-VP and PS-DVB sorbent was proposed. Favorable methodological parameters were achieved, with correlation coefficients spanning from 0.9866 to 0.9998. The LODs of the PPCPs fluctuated from 0.001 to 2 μg L −1 , while the LOQs varied from 0.002 to 5 μg L −1 . The analysis of spiked samples disclosed a methodological precision of 2.31–9.86 % and a recovery of 52.4–119 %. We utilized the established method for analyzing 14 water samples of three categories (source water, finished water and tap water) from five centralized water supply plants. A total of 24 categories encompassing 72 PPCPs were detected, with the concentrations of PPCPs manifested a marked decrease from source water to finished water and finally to tap water. Significance Our research meticulously examined the enhancement and purification effects of widely used commercial SPE cartridges and suggested the use of in-lab fabricated SPE cartridges packed with DVB-VP and PS-DVB adsorbents. We also conducted a systematic evaluation of the need to incorporate ascorbic acid and sodium thiosulfate as preservatives for PPCP measurement, in consideration of the unique characteristics of drinking water matrices, specifically, the significant concentration levels of disinfectants. Furthermore, the proposed method was effectively employed to study the presence of PPCPs in source water, finished water, and tap water collected from centralized water supply plants.
研究领域:
环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 7
·1-10
·
IF 6.232
Zhang Xue,Shen Yan-Feng,Li Xin-Xin,Yang Jin-Rong,Liu Zhao-Sheng,Huang Yan-Ping
An organic-inorganic hybrid monolithic column doped with gold nanorods (AuNRs) was prepared and evaluated for solid phase extraction (SPE) of polycyclic aromatic hydrocarbons (PAHs). Excellent dispersibility of AuNRs in binary green porogen system consisting of 1-hexyl-3-methylimidazolium tetrafluoroborate and deep eutectic solvents (DESs) was confirmed by energy dispersive spectrometry (EDS). The particle size of the resulting AuNRs (70–90 nm) was thoroughly examined by a transmission electron microscopy (TEM). The redox system including ammonium persulfate (APS) and tetramethylethylenediamine (TEMED) was used to initiate in situ polymerization at 4 °C to prepare the hybrid monolith. The mesoporous structure of the AuNR hybrid monoliths was confirmed by scanning electron microscopy (SEM) and nitrogen adsorption. With enrichment factors (EFs) of 150- to 292-fold, the developed method was successfully applied to the determination of 10 PAHs in wastewater samples. The recoveries at a spiked level were in the range 84.9 to 99.5% with limit of detections (LODs) and relative standard deviations (RSDs) ranging from 0.02 to 0.10 μg L −1 and 1.5 to 4.2%, respectively. The correlation coefficients ( R 2 ) for the calibration function obtained were better 0.9991 for the target compounds. Compared to the AuNR-free monolith, the extraction efficiency of the AuNR-incorporated monolith is more than two times higher. The results indicated that the doping of AuNRs is an effective approach to obtain the hybrid monolithic column with good separation ability for PAHs.
Graphical abstract
研究领域:
分析化学
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环境科学
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DOI
PubMed
高影响因子
Nanomaterials
·
2022
·Vol. 12
·期 13
·2213
·
IF 5.719
Yafei Hou,Xiaodan Pei,Yuancheng Wang,Luyuan Zhang,Xiaohui Wei,Hongyan Mao,Wuduo Zhao,Shusheng Zhang,Wenfen Zhang
The aromatic structure and the rich nitrogen content of polymers based on covalent triazine-based frameworks (CTF) and their unique hydrophilic-lipophilic-balanced adsorption properties make them promising candidates for an adsorbent that can be used for sample pretreatment. Herein, a new covalent triazine-based framework (CTF-DBF) synthesized by a Friedel–Crafts reaction was used for the determination of the content of nucleotides in commercial infant formula. It was shown that the synthetic materials had an amorphous microporous structure, a BET surface area of up to 595.59 m2/g, and 0.39 nm and 0.54 nm micropores. The versatile adsorption properties of this material were evaluated by quantum chemistry theory calculations and batch adsorption experiments using five nucleotides as probes. The quantum chemistry results demonstrated that CTF-DBF can participate in multiple interactions with nucleotides. All the analyses performed present good linearity with R2> 0.9993. The detection limits of targets ranged from 0.3 to 0.5 mg/kg, the spiked recoveries were between 85.8 and 105.3% and the relative standard deviations (RSD, n = 6) were between 1.1 and 4.5%. All these results suggest that this versatile CTF-DBF has great potential for sample pretreatment.Keywords:covalent triazine-based frameworks;solid-phase extraction;nucleotides
研究领域:
分析化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2023
·
IF 4.3
Dian-Bing Zhou,Hai-Tao Zhu,Yu-Zhu Hou,Gui-Lan Shen,Can Shi,Ya-Jie Zhu,Ya-Bing Xiao,Wei Song,Yu-Xin Liu,Fang Han,Ping Zheng,Xiao-Feng Yu
The conventional method for the determination of heavy metals in food is acid digestion followed by atomic absorption spectrometry or induced coupled plasma mass spectrometry . However, for high salt foods, due to the strong matrix effect, the detection results are seriously inaccurate. In this work, sulfur-functionalized magnetic metal-organic frameworks (Fe 3 O 4 @UiO-66-SH) were synthesized by coating Fe 3 O 4 nanospheres with sulfydryl-functionalized UiO-66. The Fe 3 O 4 @UiO-66-SH possesses both the magnetic properties of Fe 3 O 4 and the diverse properties of metal-organic framework (MOF) in one material, which has the superiority of high surface area, easy-operation and strong adsorb ability with Pb (II) and Cd(II), is used to separate and determine Pb (II) and Cd(II) in high salt foods by magnetic solid phase extraction-induced plasma mass spectrometry. The detection limits (LODs) for Pb (II) and Cd(II) were 0.17 and 0.21 µg/kg, respectively, and the quantification limits (LOQs) were 0.56 and 0.66 µg/kg. Analyzing the certified reference material of soy sauce (CFAPA-QC1728–4, P41839) and estimating the spiked recoveries proved the accuracy and precision of the proposed method. The determined values agreed well with the reference values, and the recoveries for spiking sample varied from 85.8–100.5%.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Xiwen Liu,Qingkun Hu,Yuanjun Tong,Nan Li,Sai Ouyang,Huangsheng Yang,Jianqiao Xu,Gangfeng Ouyang
Solid-phase extraction (SPE) is a popular technique for environmental sample pretreatment . However, SPE usually requires complex sample pretreatment processes, which is time-consuming and inconvenient for real-time and on-site monitoring. Herein, a solvent-free, rapid, and user-friendly SPE device was developed by coating the polydimethylsiloxane (PDMS)/divinylbenzene (DVB) sorbent on the inner wall of a sample bottle. The extraction process and desorption process were both carried out in the bottle. The analytes trapped in the sorbent were thermally desorbed and simultaneously sucked out from the bottle by an air sampling tube equipped on field-portable GC-MS. Different to previous work, the sample pretreatment process didn’t require any complicated and time-consuming steps, such as centrifugation or filtration. The total analysis time for each sample was less than 25 min, which was feasible for rapid on-site detection, and thus avoided the losses and contamination of samples in conventional sample storage and transportation processes. Under optimal conditions, the proposed SPE method exhibited wide linear ranges, low detection limits (0.010–0.036 μg L −1 , which were much lower than the maximum levels restricted by the US Environmental Protection Agency and the Chinese GB3838-2002 standard), good intra-bottle repeatability (6.13–7.17%, n = 3) and satisfactory inter-bottle reproducibility (4.73–6.47%, n = 3). Finally, the method was successfully applied to the rapid detection of BTEX in the field. The recoveries of BTEX in spiked water samples ranged from 89.1% to 116.2%. This work presents a novel SPE approach for rapid on-site monitoring in water samples.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
PubMed
高影响因子
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
·
2015
·
IF 0.754
Liang-Liang HUANG,Yan HUANG,Yan-Kai CHEN,Yun-Hua DING,Wei-Feng ZHANG,Xiao-Jing LI,Xiao-Ping WU
A simple and green method for the determination of trace bisphenol A (BPA) was established by coupling supported ionic liquid solid-phase extraction to β -cyclodextrin modified ionic liquids carbon paste electrode-based electrochemical detection (SILs-SPE-ED). The synthesized imidazolium ionic liquids modified styrene type macroporous resin was used as adsorbent for SPE of BPA. The experimental parameters that affected the extraction efficiency were investigated and optimized. Dynamic adsorption test showed that the maximum adsorption capacity of BPA on the SILs-SPE cartridge was 10.1 mg g −1 , and the enrichment factor was 40. The calibration curve showed a good linearity between the anodic current and the BPA concentration in the range of 1.0 × 10 −8 −1.0 × 10 −6 M. The detection limit was 4.16 nM (equal to 0.95 μg L −1 ). The SILs-SPE-ED method, with the advantages including high sensitivity and good practicability, was applied to the analysis of real water and plastic samples, and the results agreed well with HPLC method.
研究领域:
分析化学
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环境科学
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2017
·
IF 6.32
Boyin Yan,Zhiquan Liu,Rui Huang,Yongpeng Xu,Dongmei Liu,Tsair-Fuh Lin,Fuyi Cui
There is a serious dispute on the existence of β-N-methylamino-l-alanine (BMAA) in water, which is a neurotoxin that may cause amyotrophic lateral sclerosis/Parkinson’s disease (ALS/PDC) and Alzheimer’ disease. It is believed that a reliable and sensitive analytical method for the determination of BMAA is urgently required to resolve this dispute. In the present study, the solid phase extraction (SPE) procedure and the analytical method for dissolved BMAA in water were investigated and optimized. The results showed both derivatized and underivatized methods were qualified for the measurement of BMAA and its isomer in natural water, and the limit of detection and the precision of the two methods were comparable. Cartridge characteristics and SPE conditions could greatly affect the SPE performance, and the competition of natural organic matter is the primary factor causing the low recovery of BMAA, which was reduced from approximately 90% in pure water to 38.11% in natural water. The optimized SPE method for BMAA was a combination of rinsed SPE cartridges, controlled loading/elution rates and elution solution, evaporation at 55 °C, reconstitution of a solution mixture, and filtration by polyvinylidene fluoride membrane. This optimized method achieved > 88% recovery of BMAA in both algal solution and river water. The developed method can provide an efficient way to evaluate the actual concentration levels of BMAA in actual water environments and drinking water systems.
研究领域:
环境科学
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
SPECTROSCOPY LETTERS
·
2017
·
IF 0.794
Xiaohuan Zang,Qingyun Chang,Weiqian Liang,Chun Wang,Zhi Wang
A magnetic hydroxypropyl-β-cyclodextrin-functionalized reduced graphene oxide was synthesized and used as a magnetic solid-phase extraction adsorbent for the enrichment of cadmium from water and food samples before its determination by flame atomic absorption spectrometry. The effects of pH, amount of adsorbent, extraction time, desorption condition, and coexisting ions on the extraction efficiency were investigated and optimized. Under the optimal conditions, the limit of detection was 0.23 µg L−1 for water samples and 0.015 µg g−1 for food samples, respectively. The linear range was between 0.50 and 100.0 µg L−1 with a good correlation coefficient of 0.9986 in water samples, and between 0.050 and 5.0 µg g−1 with a correlation coefficient of 0.9975 in food samples. The method recoveries for the spiked samples were in the range of 87.5–102.4%, with the relative standard deviations ranging from 4.7% to 6.2% and enrichment factors ranging from 38 to 41, respectively. The adsorbent could be reused over 50 times without a significant change of extraction capability. The established method provides a promising environmentally friendly alternative for the determination of cadmium in complex matrix samples with no need of additional chelating reagents during the extraction process.
研究领域:
分析化学
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环境科学
✓ 已验证
DOI
高影响因子
LUMINESCENCE
·
2023
·Vol. 38
·期 11
·1938-1945
·
IF 2.9
Jiayan Shen,Long Li,Kehan Xu,Kaijun Wang,Yiping Du,Ting Wu,Huipeng Deng
A rapid and sensitive strategy was proposed for the detection of fluoranthene (FL), which is a polycyclic aromatic hydrocarbon (PAH), in water samples. In this work, syringe solid-phase extraction (SPE) combined with solid-phase fluorescence spectrometry was used to determine FL in PAHs polluted environmental samples. The fluorescence signals were directly monitored on the membrane surface after FL was enriched by syringe SPE. Under the optimal conditions, the proposed method showed a linear relationship in the concentration range 2–50 μg/L with a correlation coefficient ( R 2 ) of 0.998, and the limit of detection was 0.143 μg/L. The recoveries varied from 93.47% to 109.81% in the actual samples, with the relative standard deviations ( n = 3) ranging from 2.06% to 6.32%. According to the results, the established method can be applied in the field of rapid detection as it is fast, simple, portable, and highly sensitive, and has strong anti-interference.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2023
·
IF 4.3
Mohammad Nazari Kalojeh,Roghayeh Hassanpour Sabet,Mir Ali Farajzadeh,Mohammad Reza Afshar Mogaddam,Elnaz Marzi Khosrowshahi,Mustafa Tuzen
A dispersive solid phase extraction procedure was established for the extraction of some pesticides from fruit juices and then it was combined with dispersive liquid-liquid microextraction for more enrichment of the analytes. For this purpose, 40 mg of zeolitic imidazolate framework-carbon dot composite was dispersed into the sample solution as the sorbent via vortex agitation. After that, the sorbent was collected by centrifugation and the supernatant was wasted. Then, 1 mL of a water-soluble organic solvent (acetone) was added onto the sorbent as the elution solvent. After desorption of the analytes from the sorbent surface, the eluate was mixed with a water-immiscible organic solvent (1,1,2-trichloro-1,2,2 trifluoroethane) at µL-level (45 µL) and the mixture was quickly injected into 5 mL deionized water. The resulting cloudy mixture was centrifuged and 1 µL of the sedimented phase was injected into a gas chromatography-flame ionization detection system. After the optimization of the method, its validation was evaluated. The data showed that the limits of detection and quantification obtained by this method were in the ranges of 0.22–0.72 and 0.73–2.40 ng mL −1 , respectively. The plotted calibration curves were linear in the range of 0.73–1000 µg L −1 for all analytes. High enrichment factors (375−445), and extraction recoveries (75–89%), and negligible matrices effect were obtained for the investigated analytes by the introduced method. Also, the obtained data showed that all samples were free of the analytes.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
高影响因子
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