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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY · 2022 · IF 2.731

RETRACTED ARTICLE: Occurrence and spatial distribution of plasticizers in aquatic environment of Guangzhou, China

Jiancong Wang,Xiufeng Duan,Hanbing Du,Xiaoyun Yang,Hanhong Xu

Statement of RetractionWe, the Editor and Publisher of the journal International Journal of Environmental Analytical Chemistry, have retracted the following article: Jiancong Wang, Xiufeng Duan, Hanbing Du, Xiaoyun Yang, and Hanhong Xu (2022) Occurrence and spatial distribution of plasticizers in aquatic environment of Guangzhou, Chinadoi.org/10.1080/03067319.2022.2128796It has come to our attention that this article contained incorrect data in the sample preparation section. The Authors contacted us to inform of this error and requested for the article to be retracted.We have been informed in our decision-making by our policy on publishing ethics and integrity and the COPE guidelines on retractions. The retracted article will remain online to maintain the scholarly record, but it will be digitally watermarked on each page as ‘Retracted’.

CAS / MDL: 1318-02-1 67-66-3
研究领域: 环境科学 · 化学分析
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MOLECULES · 2019 ·Vol. 24 ·期 15 ·2761 · IF 3.06

Matrix-Induced Sugaring-Out: A Simple and Rapid Sample Preparation Method for the Determination of Neonicotinoid Pesticides in Honey

Wenbin Chen,Siyuan Wu,Jianing Zhang,Fengjie Yu,Jianbo Hou,Xiaoqing Miao,Xijuan Tu

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.

研究领域: 分析化学 · 食品科学
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ANALYTICA CHIMICA ACTA · 2021 · IF 6.558

Ultrasound-assisted electromembrane extraction with supported semi-liquid membrane

Qianqian Shang,Hang Mei,Xinrui Feng,Chuixiu Huang,Stig Pedersen-Bjergaard,Xiantao Shen

Electromembrane extraction (EME), involving the migration of charged analytes across a supported liquid membrane (SLM) with an external power supply, is a promising sample preparation method in analytical chemistry . However, the presence of boundary double layers at the SLM/solution interfaces often restricts extraction efficiency. To avoid this, the current work proposed an ultrasound-assisted EME (UA-EME) method based on a novel type of supported semi-liquid membrane (SsLM). The characterizations showed that the SsLM was stable under ultrasound conditions. Ultrasound was found to reduce the boundary double layers and thus increase the mass transfer. Major operational parameters in UA-EME including ultrasound power density, temperature, applied voltage and extraction time were optimized with haloperidol , fluoxetine , and sertraline as model analytes. Under the optimal conditions, extraction recoveries of model analytes in water samples were in the range of 66.8%–91.6%. When this UA-EME method was coupled with LC-MS/MS for detection of the target analytes in human urine samples, the linear range of the analytical method was 10–1000 ng mL −1 , with R 2  > 0.997 for all analytes. The limits of detection (LOD) and limits of quantification (LOQ) were in the range of 1.7–2.1 ng mL −1 and 5.7–6.7 ng mL −1 , respectively. The UA-EME expands the application field of ultrasound chemistry and will be very important in development of stable and fast sample preparation systems in the future.

研究领域: 分析化学 · 超声化学 · 药物分析
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ANALYTICAL LETTERS · 2024 · IF 1.6

Pouring and Curing for Sample Preparation Technology for the Analysis of the Silicon-Aluminum Ratio of Molecular Sieves by Energy Dispersive X-Ray Fluorescence (EDXRF)

Qing Shan,Yangxue Luo,Xinlei Zhang,Zhanpeng Zhang,Wenbao Jia,Yongsheng Ling,Daqian Hei,Jiandong Zhang,Chao Shi,Jiehua Bao

The silicon-aluminum ratio of the molecular sieves is a crucial control index for the quality of synthetic molecular sieves. Here a fast, simple and reliable sample preparation method, referred to as pouring and curing method, is described for determining the silicon-aluminum ratio of high silicon molecular sieves by energy dispersive x-ray fluorescence (EDXRF). Resin is used as the carrier with the addition of a curing agent, so that the sample powder is embedded in the resin matrix. By measuring sixteen random positions of the same cured sample, the homogeneity of the sample was evaluated to ensure the stability of the results. A double logarithmic calibration curve of the analysis line ratio and the corresponding concentration ratio of silicon and aluminum was established according to the binary ratio method. The results by EDXRF and inductively coupled plasma-optical emission spectrometer (ICP-OES) were compared with a relative standard error from 2.934 to 6.777%. The good precision shows that the pouring and curing method is a suitable for measuring the silicon-aluminum ratio of molecular sieves.

CAS / MDL: 1344-28-1
研究领域: 材料科学 · 分析化学
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CHEMICAL ENGINEERING JOURNAL · 2024 · IF 13.3

Protonic and electronic hole conductivity of grain interior and grain boundaries in BaZr0.9Y0.1O3-δ: Effect from sample processing

Lulu Jiang,Donglin Han

BaZr 0.9 Y 0.1 O 3-δ (BZY10) is a popular composition for the electrolyte in protonic ceramic cells, due to its relatively high proton conductivity, excellent chemical stability, and good compatibility with NiO negatrode substrate during high temperature co-sintering. The microstructure of BZY10 is highly dependent on sample processing, leading to large discrepancy of the electrochemical performance of BZY10 in literature. In this work, three BZY10 samples were prepared by different sample processing and sintering conditions, and the grain interior (bulk) and grain boundary partial conductivities of protons and holes were separated. The sintering processes influenced the transport properties of pristine BZY10 samples significantly, and longer sintering time at high temperature (1650 – 1700 °C) leads to lower proton conductivity in both bulk and grain boundary. However interestingly, longer sintering time resulted in higher ionic transport number of bulk conduction, but lower ionic transport number of grain boundary conduction, possibly due to increasing Ba-deficiency in bulk by longer annealing at high temperature. Besides, adding ZnO into BZY10 decreased the proton conductivity in both bulk and grain boundary, but its ionic transport number of bulk conduction increases. A further analysis based on the theory of space charge layer indicated that adding ZnO leaded to decreased Schottky barrier height in the grain boundary core, and the highest Schottky barrier height was observed in the pristine sample which was sintered for longer time. The results obtained in this work suggest a potential strategy to regulate the transport properties of BZY10 by choosing appropriate approaches for sample processing to control the microstructure and local composition of the polycrystalline BZY10 ceramic electrolyte.

研究领域: 材料科学 · 固体物理 · 能源科学
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ACS Applied Materials & Interfaces · 2016 · IF 7.145

Synthesis of Polyethylenimine Functionalized Mesoporous Silica for In-Pipet-Tip Phosphopeptide Enrichment

Gang-Tian Zhu,Xiao-Mei He,Sheng He,Xi Chen,Shu-Kui Zhu,Yu-Qi Feng

Synthesis of functionalized mesoporous silica material with large particle size remains a chanllenge. In this work, polyethylenimine (PEI) functionalized mesoporous silica (PFMS) with particle size as large as 100 μm was successfully synthesized by a facile method. In the synthesis process, PEI served as four roles simultaneously, including functionalized reagent, alkaline catalyst, template for particle formation, and pore-structure-directing agent. The surface areas of the products were higher than 260 m2/g. Benefiting from the large particle size and high surface area, PFMS was packed in a pipet tip to fabricate a convenient and miniaturized solid phase extraction apparatus for sample preparation. Additionally, based on the extremely abundant basic sites in the organic units of PFMS, the in-pipet-tip system was used as an anion-exchanger for phosphopeptide enrichment. The specificity of the developed method was investigated by capture of phosphopeptides from tryptic digests of standard protein mixtures, tryptic digests of nonfat milk, and human serum. Furthermore, the method was utilized to analyze phosphopeptides in tryptic digests of rat brain lysate, and 2251 unique phosphopeptides were successfully detected.

CAS / MDL: 13463-67-7 9002-98-6
研究领域: 分析化学 · 材料科学 · 蛋白质组学
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CHINESE CHEMICAL LETTERS · 2018 · IF 2.631

A membrane separation technique for optimizing sample preparation of MALDI-TOF MS detection

Zengnan Wu,Ning Xu,Weiwei Li,Jin-Ming Lin

The performance of matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS) is frequently compromised by the high limited of detection, heterogeneous distribution of matrix and analyte deposits and time-consuming drying time during the conventional drop drying procedure. Here, we describe a method based on membrane separation technology to assist in the drying of nanomaterials to rapidly make homogeneous sample spots and to enhance the mass signal. We demonstrate that the sample can be dried evenly in a few seconds and MS signal can be greatly optimized by using membrane separation technology. Enrichment with nanomaterials greatly enhances analyte signal strength while membrane separation method avoids the time-consuming requirements of searching for “sweet spots”.

CAS / MDL: 308068-56-6
研究领域: 分析化学 · 质谱技术 · 纳米技术
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MOLECULES · 2021 ·Vol. 26 ·期 8 ·2350 · IF 4.412

Micro Salting-Out Assisted Matrix Solid-Phase Dispersion: A Simple and Fast Sample Preparation Method for the Analysis of Bisphenol Contaminants in Bee Pollen

Jianing Zhang,Fengjie Yu,Yunmin Tao,Chunping Du,Wenchao Yang,Wenbin Chen,Xijuan Tu

In the present work, a novel sample preparation method, micro salting-out assisted matrix solid-phase dispersion (μ-SOA-MSPD), was developed for the determination of bisphenol A (BPA) and bisphenol B (BPB) contaminants in bee pollen. The proposed method was designed to combine two classical sample preparation methodologies, matrix solid-phase dispersion (MSPD) and homogenous liquid-liquid extraction (HLLE), to simplify and speed-up the preparation process. Parameters of μ-SOA-MSPD were systematically investigated, and results indicated the significant effect of salt and ACN-H2O extractant on the signal response of analytes. In addition, excellent clean-up ability in removing matrix components was observed when primary secondary amine (PSA) sorbent was introduced into the blending operation. The developed method was fully validated, and the limits of detection for BPA and BPB were 20 μg/kg and 30 μg/kg, respectively. Average recoveries and precisions were ranged from 83.03% to 94.64% and 1.76% to 5.45%, respectively. This is the first report on the analysis of bisphenol contaminants in bee pollen sample, and also on the combination of MSPD and HLLE. The present method might provide a new strategy for simple and fast sample preparation of solid and semi-solid samples.Keywords:sample preparation;matrix solid-phase dispersion;salting-out;homogenous liquid-liquid extraction;bisphenol;bee pollen

研究领域: 分析化学 · 环境科学
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ANALYTICAL CHEMISTRY · 2017 · IF 6.32

Spatial Profiling of Gibberellins in a Single Leaf Based on Microscale Matrix Solid-Phase Dispersion and Precolumn Derivatization Coupled with Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry

Ting Deng,Dapeng Wu,Chunfeng Duan,Xiaohui Yan,Yan Du,Jun Zou,Yafeng Guan

A spatial-resolved analysis method for profiling of gibberellins (GAs) in a single leaf was developed on the basis of microscale sample preparation and precolumn derivatization coupled with ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The proposed microscale sample preparation was based on modified matrix solid-phase dispersion (MSPD) method, in which the plant sample (<1 mg) and C18 sorbent were ground together in one microcentrifuge tube, and then extraction solvent was added followed by centrifugation. In this protocol, the grinding, extraction, and purification were performed in one microcentrifuge tube without any sample transfer step, resulting in an obvious decrease in sample loss. Moreover, a new derivatization reagent, 3-bromopropyltrimethylammonium bromide (BPTAB), was used to further enhance the signal intensities of GAs on MS by 3–4 orders of magnitude, which was much higher than the reported derivatization reagents for GAs such as bromocholine bromide and 3-bromoactonyltrimethylammonium bromide. The present method showed high sensitivity (minimum detectable amount (MDA) of 10.1–72.3 amol for eight GAs) and low sample consumption (down to 0.30 mg FW). Under the optimized conditions, the distribution of GA19 in a single Arabidopsis thaliana leaf was profiled with a spatial resolution of 2 × 2 mm2.

CAS / MDL: 541-46-8
研究领域: 植物学 · 分析化学
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MOLECULES · 2023 ·Vol. 28 ·期 14 ·5307 · IF 4.6

Determination of Lincomycin in Milk Using Cu-Based Metal-Organic Framework Adsorbent and Liquid Chromatography-Tandem Mass Spectrometry

Hanle Li,Jinhai Wu,Jialei Bai,Jianhu Wu,Jin Wu

Antibiotic drug residues can adversely affect the human body. Lincomycin is a common veterinary drug that can form residues in foods of animal origin. However, the detection of trace residue levels of lincomycin residues in real samples is challenging. Here, a simple solid phase extraction (SPE) method was developed for the enrichment of lincomycin from cow milk samples before its detection by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The adsorbent used in the SPE was a Cu-based metal-organic framework (Cu-MOF) prepared by the solvothermal synthesis approach. The prepared MOFs were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffractometry (XRD), differential thermogravimetric analysis (TG-DTA), and N2 adsorption-desorption experiments. The adsorption capacity (adsorption equilibrium, extraction time, pH), and elution solvent parameters were investigated. Under the optimized conditions of the HPLC-MS/MS method, lincomycin was detected in the linear range of 10–200 g/L with a detection limit of 0.013 ng/mL. Commercial milk samples were spiked with lincomycin, and a recovery rate between 92.3% and 97.2% was achieved. Therefore, the current method can be successfully applied for the enrichment and determination of lincomycin from milk samples.Keywords:Cu-based metal-organic framework;liquid chromatography-tandem mass spectrometry;sampling preparation technique;solid-phase extraction;lincomycin

CAS / MDL: 554-95-0
研究领域: 分析化学 · 食品科学 · 兽医学
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JOURNAL OF NEUROSCIENCE METHODS · 2025 · IF 2.3

Comparative evaluation of cerebral tissue pretreatment strategies for metabolomics using UHPLC-high-resolution mass spectrometry

Fang Guo,Xiaoxue Zhou,Yudie Ning,Tingli Qv,Jieping Lv,Tao Wang,Zhiwen Wei

Background The cerebrum, as the most complex human organ, contains diverse metabolites vital for understanding brain functions, diseases, drug effects, and addiction. Its liquefiable nature makes swift preparation crucial to preserve metabolic profiles, with physical homogenization needed to release metabolites. To determine the optimal preparation procedures for cerebrum samples for high-resolution mass spectrometry in metabolomics, we evaluated four homogenization techniques and three extraction protocols using UHPLC-HRMS. New method A combination of dry grinding and monophasic extraction was identified as an optimized sample preparation approach for cerebrum metabolomics. Results The number of feature peaks, coefficient of variation (CV) of peak areas, and peak areas were compared to evaluate the coverage, reproducibility, and sensitivity of the methods. The dry grinding method detected the most feature peaks among four methods of homogenization, and the peak areas obtained were superior to other homogenization methods. In terms of extraction methods, there was no significant difference in peak areas (except for tyrosine) between monophasic and two-step extraction methods (p > 0.05), both of which were higher than the biphasic extraction method (p < 0.05). Additionally, the reproducibility of the monophasic extraction method was significantly better than the other two methods. Comparison The dry grinding and monophasic extraction approach demonstrated excellent compatibility with UHPLC-HRMS, offering broader metabolite coverage and superior performance compared to existing methods. Conclusions The dry grinding and monophasic extraction method is recommended for cerebrum metabolomics, providing enhanced metabolite coverage, reproducibility, and adaptability for high-resolution mass spectrometry studies.

CAS / MDL: 64-18-6
研究领域: 神经科学 · 代谢组学 · 分析化学 · 质谱分析
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Food Analytical Methods · 2023 ·Vol. 16 ·期 5 ·909-917 · IF 2.9

Determination of Seven Biogenic Amines in Tuna with High-Performance Liquid Chromatography Coupled to Electrospray Ionization Ion Mobility Spectrometry

Xu Yanfen,Lu Ying,Yu Jianna,Liu Wen,Jing Guoxing,Li Wenshan,Liu Wenjie

Tuna is one of the most popular fish and therefore among the most commercially valuable seafood. However, inadequate refrigeration during the whole supply chain causes serious economic loss and food poisoning. One important result of tuna spoilage is the accumulation of biogenic amines such as histamine, which can be used as a sensitive indicator for Tuna freshness. Thus, the development of rapid, sensitive, and economic analytical methods for biogenic amines in Tuna is highly desired. This research developed a method that combines high-performance liquid chromatography (HPLC) and electrospray ionization ion mobility spectrometry (ESI-IMS) to detect 7 kinds of biogenic amines including tryptamine, tyramine, spermidine, cadaverine, β-phenylethylamine, putrescine, and histamine in tuna. The limit of detections (LODs) for 7 biogenic amines are 0.01, 0.02, 0.02, 0.17, 0.03, 0.04, and 0.15 mg L −1 respectively. The linear range of histamine and spermidine is 2–100 mg kg −1 , and the linear range of other biogenic amines is 0.5–10 mg L −1 . The recoveries of biogenic amines are between 69.39 and 112.65%. Compared to the traditional HPLC-based analytical method, the proposed method does not involve any derivatization steps, which greatly decreased the sample preparation time and cost. Another advantage of the developed method is the supplementary separation to the HPLC, in which coeluted biogenic amines can clearly be separated in the ion mobility dimension. The proposed method is applied to determining the concentration of biogenic amines in tuna storage, which showed that this method can quickly and accurately monitor the changes of biogenic amines in tuna during storage.

研究领域: 分析化学 · 食品科学 · 生物化学
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