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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2025 · IF 6.2

Identification of Polyamines in Human Milk, Formula Milk, and Other Dairy Products: a Special Method Based on Precolumn Derivatization, Double-Florisil Purification, and Gas Chromatography–Triple Quadrupole Mass Spectrometry

Li Wang,Yating Sun,Linjing Dong,Yuanyuan Li,Qin Zhang,Ye Ding,Jieshu Wu,Zhixu Wang

Polyamines in human milk are essential for the rapid growth and development of neonates and infants. However, the concentrations of polyamines in human milk have not been well characterized and the special methods for detecting polyamines in human milk, formula milk, or other dairy products remain largely unavailable to date. In this study, an accurate and sensitive method based on trifluoroacetic acid anhydride (TFAA) derivatization, double solid-phase extraction (SPE) purification, and gas chromatography–triple quadrupole mass spectrometry (GC-QqQ MS) was established for the evaluation of polyamines in human milk, formula milk, and other dairy products. High coefficients of determination for internal calibration curves were obtained (R2 > 0.99). Low limits of detection (5.0, 1.0, and 0.5 nmol/dL) and limits of quantification (10.0, 3.0, and 1.0 nmol/dL) for putrescine, spermidine, and spermine, respectively, were also achieved. The precision (expressed as relative standard deviation, RSD < 9.0%) and recovery rates (78.3–108.4%) were satisfactory. Spermidine and spermine in human milk were found significantly higher than those in formula milk and commercial cow’s milk. The difference of polyamine content in human milk and infant formula should be paid attention to, particularly when infant formula is used as a complete replacement for human milk.

CAS / MDL: 76-05-1
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FOOD CHEMISTRY · 2024 · IF 8.5

Covalent organic framework-functionalized magnetic MXene nanocomposite for efficient pre-concentration and detection of organophosphorus and organochlorine pesticides in tea samples before gas chromatography–triple quadrupole mass spectrometry analysis

Liushan Jiang,Guangyu Dong,Denghao Song,Wenjing Liu,Xiaodie Geng,Dejing Meng,Linchun Nie,Jiawei Liao,Qingxiang Zhou

In this study, a hydrophobic covalent organic framework-functionalized magnetic composite (CoFe 2 O 4 @Ti 3 C 2 @TAPB−TFTA) with a high specific area with 1,3,5-tris(4-aminophenyl)benzene (TAPB) and 2,3,5,6-tetrafluoroterephthalaldehyde (TFTA) was designed and synthesized through Schiff base reaction. An efficient magnetic solid-phase extraction method was established and combined with gas chromatography–triple quadrupole mass spectrometry to sensitively determine 10 organochlorine and organophosphorus pesticides in tea samples. The established method exhibited good linearity in the range of 0.05–120 μg/L and had low limits of detection (0.013–0.018 μg/L). The method was evaluated with tea samples, and the spiked recoveries of pesticides in different tea samples reached satisfactory values of 85.7–96.8%. Moreover, the adsorption of pesticides was spontaneous and followed Redlich–Peterson isotherm and pseudo-second-order kinetic models. These results demonstrate the sensitivity, effectiveness, and reliability of the proposed method for monitoring organochlorine and organophosphorus pesticides in tea samples, providing a preliminary basis for researchers to reasonably design adsorbents for the efficient extraction of pesticides.

CAS / MDL: 919-30-2
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ENERGY CONVERSION AND MANAGEMENT · 2024 · IF 9.9

An eco-friendly system of thermally regenerative battery-driven electrochemical CO2 reduction: In-situ harvesting of low-grade heat as electrical power for reducing CO2 emissions of flue gas

Si Li,Zhenchong Xiao,Yu Shi,Liang Zhang,Jun Li,Qian Fu,Xun Zhu,Qiang Liao

To realize the utilization of power energy from thermally regenerative batteries and treat flue gas, an eco-friendly coupled system of thermally regenerative battery-driven electrochemical reduction of carbon dioxide is proposed. This system recovers low-grade waste heat for electrical power while in-situ utilization for carbon dioxide reduction. The results show that carbon nanotubes-loaded silver catalyst enhances electrochemical carbon dioxide reduction performance due to increased active sites exposure. Output voltage and maximum power correlate linearly with the number of cell pairs in the thermally regenerative battery stack. Operating with 4 cell pairs, the eco-friendly coupled system achieves an average carbon monoxide Faradaic efficiency of 76.6 % and an average carbon monoxide Faradaic current density of 5.4 mA cm −2 . A minimum of 3 cell pairs is necessary for system operation. The increase of cell pairs in a certain range is beneficial for the performance improvement of electrochemical reduction of carbon dioxide. The eco-friendly coupled system attains an average Faradaic efficiency of 89.4 % and an average carbon monoxide Faradaic current density of 17.8 mA cm −2 with 8 cell pairs. This coupled system indicates a feasible and promising way to simultaneously reduce the emission of low-grade waste heat and carbon dioxide in flue gas without additional inputs.

CAS / MDL: 15418-29-8
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ANALYST · 2012 ·Vol. 137 ·期 22 ·5411-5419 · IF 4.23

Metal–organic framework MIL-53(Al) as a solid-phase microextraction adsorbent for the determination of 16 polycyclic aromatic hydrocarbons in water samples by gas chromatography–tandem mass spectrometry

Xiang-Feng Chen,Hao Zang,Xia Wang,Jian-Guang Cheng,Ru-Song Zhao,Chuan-Ge Cheng,Xiao-Qing Lu

In this paper, the potential applications of metal–organic framework (MOF) materials as fiber coatings for the solid-phase microextraction (SPME) of polycyclic aromatic hydrocarbons (PAHs) in water samples were explored. Fibers coated with MIL-53(Al, Cr, Fe) materials were fabricated by an adhesive method for SPME. The quantitation was performed by gas chromatography–tandem mass spectrometry (GC–MS/MS) using the multiple reaction monitoring mode. Among the three MIL-53(M) coatings, MIL-53(Al) showed the highest extraction efficiency towards PAHs under the current fabrication procedure. Under optimized conditions, the MIL-53(Al)-coated fiber showed good precision (relative standard deviation <12.5%), low detection limits (0.10 ng L−1 to 0.73 ng L−1, S/N = 3), and good linearity (R2 > 0.98) for aqueous solutions containing 16 PAH . The fiber also offered high thermal and chemical stability. The method developed based on MIL-53(Al) SPME–GC–MS/MS was successfully applied in the analysis of real water samples. Based on the simulation results, the PAHs were adsorbed on MIL-53(Al) primarily through the hydrophobic and π–π interactions between PAHs and the organic linker of the material. The results presented in this paper indicate that water-stable MOF materials have great potential for the SPME of aromatic compounds in water samples.

CAS / MDL: 100-21-0
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DESALINATION · 2025 · IF 9.8

Efficient recovery of lithium from the reverse osmosis concentrate of shale gas wastewater treatment: Adsorption performance and mechanism of Al-doped manganese-based adsorbent particles prepared via hydrophilic modification

Xin Li,Xifan Li,Quanxun Liang,Guijing Chen,Wenjie Wang,Jin Bao,Jiawang Qin,Shun Tang,Xiao Lin,Alberto Tiraferri,Baicang Liu

The growing demand for lithium in energy storage batteries has driven interest in extracting lithium from shale gas wastewater as a sustainable alternative to traditional mining. To address challenges such as high cycling loss of adsorbent powder and complex operational procedures, this study developed adsorbent spheres by pelletizing Al-modified H 1.33 Mn 1.67 O 4 powder with polyvinyl chloride (PVC) as the skeleton material, and introducing cellulose acetate (CA) or Pluronic F127 as hydrophilic modifiers. CA-modified powder exhibited superior mechanical stability, internal porosity, and hydrophilicity. These properties reduced interference from organic matter and allowed a lithium adsorption capacity of 20.2 mg/g, surpassing the 18.8 mg/g capacity of unmodified PVC particles. Adsorption behavior followed the Freundlich isotherm model, while pseudo-second-order kinetics indicated that multi-step and multi-layer chemisorption governed lithium uptake. In fixed-bed filtration experiments, the optimal empty bed contact time (EBCT) was determined to be 40 min, leading to an adsorption saturation bed volume more than 40 times the empty bed volume. Desorption enrichment provided lithium concentrations of approximately 200 mg/L. The adsorbent maintained its adsorption capacity over 10 adsorption-desorption cycles, with manganese dissolution losses below 0.3 % and in some cases as low as 0.2 %. These findings confirm the durability and efficacy of the novel composite adsorbent in lithium recovery, offering a significant step toward more efficient and sustainable lithium extraction from treated shale gas wastewater.

CAS / MDL: 9004-35-7
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Journal of Environmental Chemical Engineering · 2020 · IF 4.3

Integrating anodic membrane diffusion/biodegradation with UV photolysis, Adsorptive oxidation by activation of peroxymonosulfate over activated carbon fiber based photo cathode in one reactor system for removing toluene gas

Qiyuan Chen,Lifen Liu

Emissions of volatile organic compounds (VOCs) air pollutants adversely affected human health and air quality. A novel reactor is designed by a bio-anode chamber with a PVDF/CFC diffusion membrane module and a catalytic air cathode chamber with persulfate and activated carbon fiber (ACF) based photocathode . Peroxysulfate is activated to generate oxidizing species that promote toluene removal and oxidation together with UV photolysis and photo-electrochemical catalysis. This new reactor as air pollution control technique is able to continuously remove toluene gas from an air stream that sequentially flows through firstly the cathode chamber where UV photolysis, photo-electrochemical (PEC) oxidation are integrated with activation of peroxymonosulfate (PMS), then flows through the bio-anode chamber where adsorption/diffusion and biodegradation take place in microbial fuel cell (MFC). This integrated system exhibits high efficiency in toluene removal (∼95 %, ∼100 ppm toluene) with stable power output (cell voltage: 0.40 V) under UV light illumination. In addition, the existence of reactive species such as OH, O 2 − and SO 4 - radicals are confirmed by EPR tests. The results show that both ·OH and SO 4 - are involved in the toluene oxidative degradation with the addition of PMS, where SO 4 - plays a predominant role, indicating that combination of photolysis, cathodic adsorption/oxidation with anodic adsorption/diffusion and biodegradation provides a promising way for VOCs removal and simultaneous electricity generation at room temperature.

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JOURNAL OF CHROMATOGRAPHY A · 2021 · IF 4.759

Magnetic solid phase extraction of heterocyclic aromatic hydrocarbons from environmental water samples with multiwalled carbon nanotube modified magnetic polyamido-amine dendrimers prior to gas chromatography-triple quadrupole mass spectrometer

Qingxiang Zhou,Yongyong Yuan,Yi Sun,Xueying Sheng,Yayan Tong

Present study described a sensitive and efficient method for determination of heterocyclic aromatic hydrocarbons using multiwalled carbon nanotubes modified magnetic polyamido-amine dendrimers (MNPs@PAMAM-Gn@MWCNTs) as adsorbent for magnetic solid-phase extraction (MSPE) coupled with gas chromatography-triple quadrupole mass spectrometer (GC–MS/MS). Some pivotal parameters including PAMAM generation, adsorbent dosage, adsorption time, elution time and volume, pH and humic acid concentration were investigated to achieve the best adsorption efficiencies. Under the optimal conditions, 7-methylquinoline, dibenzothiophene and carbazole had good linearity in the concentration range of 0.005–20 μg L   −   1 , 9-methylcarbazole, 4-methyldibenzothiophene and 4,6-dimethyl dibenzothiophene had good linearity in the concentration range of 0.001–20 μg L   −   1 . All the correlation coefficients were higher than 0.996. The detection limits of the targets were in the range of 2.2 × 10 −4 –1.8 × 10 −3  μg L   −   1 with precisions less than 8.28% ( n  = 6). The enrichment factors were in the range of 141–147. The spiked recoveries were in the range of 87.0%-115.1% ( n  = 3). These results indicated that the method could be a reliable alternative tool for monitoring trace heterocyclic aromatic hydrocarbons in environmental water samples.

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BioScience Trends · 2018 ·Vol. 12 ·期 2 ·201-207 · IF 1.844

A simple and economical method of gas chromatography-mass spectrometry to determine the presence of 6 pesticides in human plasma and its clinical application in patients with acute poisoning

Guiyan Yuan,Rui Zhang,Xuwang Chen,Benjie Wang,Ruichen Guo

An economical, rapid, and sensitive method of gas chromatography-mass spectrometry (GC-MS) was developed and validated to determine the presence of six pesticides (dichlorvos, acetochlor, atrazine, chlorpyrifos, α-endosulfan, and β-endosulfan) in human plasma. The pesticides were extracted with acetonitrile and concentrated using anhydrous sodium sulfate. Then, the target compounds were analyzed and quantified with GC-MS using borneol as an internal standard. Separation was performed on a HP-5MS capillary column (30 m × 0.25 mm × 0.25 µm) with temperature programming. Detection was accomplished under electro-spray ionization (ESI) in selected ion monitoring (SIM) mode. Under optimized conditions, satisfactory linear ranges of 0.05-10 μg/mL were obtained for all of the analyzed pesticides. The linear correlation coefficients were greater than 0.99. The average recovery was between 86.8 and 106.5%. The inter- and intra-day precision ranged from 1.7-14.5% and 4.2-13.8%, respectively. Dichlorvos was unstable in plasma both at room temperature and when frozen. The other five pesticides were stable after storage at – 20°C for 17 days and two freeze-thaw cycles. Thirty-five plasma samples from 15 patients with acute self-poisoning were analyzed using this method. Dichlorvos was found in 13 plasma samples with a mean concentration of 0.289 μg/mL, and atrazine was found in 6 with a mean concentration of 0.261 μg/mL. Acetochlor was found in one plasma sample (0.153 μg/mL). This method is simple, reliable and cost-effective. It takes little time and does not waste solvents, and it can be used to routinely detect six pesticides in patients with acute poisoning.

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ANALYTICA CHIMICA ACTA · 2021 · IF 6.558

Tracking the environmental fate of fipronil and three of its metabolites in garlic based on sampling rate-corrected in vivo solid phase microextraction combined with gas chromatography-mass spectrometry

Tiantian Chen,Jiajia Hu,Yanyan Chen,Ying Liu,Yan Li,Hui Xu

In this study, a sampling rate-corrected in vivo solid-phase microextraction-gas chromatography-mass spectrometry method (SR- in vivo SPME-GC-MS) was constructed to simultaneously detect fipronil and three of its metabolites in garlic, and their environmental behavior was long-term monitored in in vivo mode. All of three fipronil metabolites were more difficult to degrade than the parent pesticide. The final degradation rates of the metabolites in garlic were in the range of 4.4%-25.1%, much lower than that of the parent (78.6%-85.8%). While their total residues amount was about 3 times as high as fipronil , exceeding the maximum residue limits regulated by China and the European Union. The steady-state concentrations of fipronil and its metabolites in garlic were positively correlated with the pesticide stress dose. In short, the established in vivo tracking method is efficient and convenient. The features of simple operation, fast analysis, acceptable sensitivity, non-harmful or non-lethal to plants, available repeated and long-term monitoring of the same organism make it attractive for in vivo tracking assay, it is of great significance for the guidance of rational use of fipronil and protection of food safety.

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JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY · 2022 · IF 5.895

Characterization of Warmed-Over Flavor Compounds in Surimi Gel Made from Silver Carp (Hypophthalmichthys molitrix) by Gas Chromatography–Ion Mobility Spectrometry, Aroma Extract Dilution Analysis, Aroma Recombination, and Omission Studies

Yueqi An,Li Wen,Wenrong Li,Xuezhen Zhang,Yang Hu,Shanbai Xiong

The warmed-over flavor (WOF) in surimi gels was characterized by gas chromatography–ion mobility spectrometry, aroma extract dilution analysis, aroma recombination, and omission studies. Surimi gels with different WOF levels were prepared by different gelling temperatures, and surimi gels heated at 90, 100, and 121 °C were considered as the samples with light, strong, and medium WOF, respectively. Based on the quantification and odor activity values, 14 aldehydes, 2 ketones, 3 alcohols, 2 benzene-containing compounds, 2 N-containing compounds, 3 S-containing compounds, 3 lactones, undecanoic acid, and 4-methylphenol were recombined to build a spiked model for surimi gels with the strongest WOF, which showed the highest similarity with the original sample. Finally, a triangle test involving omission of the aroma compounds from the spiked model proved that the WOF in surimi gels was attributed to (E,E)-2,4-decadienal, heptanal, octanal, nonanal, decanal, (E)-2-nonenal, (E)-2-octenal, (E)-2-decenal, (E,E)-2,4-heptadienal, 2,3-pentanedione, 2,6-dimethylpyrazine, 2-propylpyridine, benzothiazole, 2-methoxybenzenethiol, and 2-furfurylthiol.

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ACS Omega · 2023 · IF 4.1

Synthesis and Characterization of a Resin/Acrylamide-2-acrylamide-2-methylpropane Sulfonate-Diallyl Dimethyl Ammonium Chloride-N-vinyl-2-pyrrolidinone Polymer Microcapsule Gelling Agent for Oil and Gas Field Transformation

Yunfeng Liu,Lang Zhou,Yongfan Tang,Qiang Liu,Wei Li,Yan Zhang

Deep carbonate rock oil and gas reservoir is an important support for increasing oil and gas storage and production at present. The environment of ultradeep and ultrahigh-temperature reservoirs has put forward higher technical requirements for reservoir modification acid technology. Moreover, gelling acid is the main acid solution for high-temperature reservoir acidizing transformation, with a temperature resistance of no more than 180 °C, and the gelling agent is one of the key factors restricting its high-temperature resistance performance. In this paper, AM, AMPS, DMDAAC, and NVP were used as monomers, oxidants, and reducing agents to prepare a high-temperature-resistant polymer gel through polymerization. At the same time, microcapsules were prepared by in situ polymerization using epoxy resin as the wall material. The indoor performance evaluation results indicate that the gelling agent is easily soluble in high-concentration acid solution and has good viscosity increasing effect. At 180 °C and 170 s–1 shear rate, 0.8% mass fraction of the gelling agent was dissolved in 20% mass fraction of hydrochloric acid. After shearing for 60 min, the viscosity remained at about 22.45 mPa·s, demonstrating good temperature resistance and shear resistance, and its performance was superior to existing commonly used gelling agent products.

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BIOMEDICAL CHROMATOGRAPHY · 2019 ·Vol. 34 ·期 3 ·e4748 · IF 1.748

Microwave-assisted extraction (MAE) combined with gas chromatography–mass spectrometry (GC–MS) for determination of volatile small molecules to evaluate compatibility of antimicrobial peptide PL-5 spray with packaging materials

Chu Liu,Xiangyong Yu,Zhaorui Meng,Ning Zhao,Fujuan Bai,Longshan Zhao

A simple and efficient method involving microwave-assisted extraction (MAE) combined with GC–MS was established to determine 1,3-di- tert -butylbenzene (DBB), 2,4-di- tert -butylphenol (DBP), 3,5-di- tert -butyl-4-hydroxybenzaldehyde (DBHBA) for evaluating the compatibility of antimicrobial peptide PL-5 spray with drug-packaging materials. In this study, the antimicrobial peptide PL-5 spray was purified using a Welchrom C18 column, and the high-density polyethylene spray bottle with liquid collection tube was first mixed with absolute ethanol, which would be subjected to MAE for further measurement by GC–MS. Various experimental parameters were systematically optimized, and good linearities were obtained within the range of 0.05–1.00 μg/mL for DBB and DBHBA and 0.50–10.00 μg/mL for DBP, with limits of detection (LODs) of 0.99 ng/mL (DBB), 16.34 ng/mL (DBP), and 1.64 ng/mL (DBHBA). Satisfactory recoveries that ranged from 96.0% to 107.2% were acquired, and the relative standard deviation was ≤ 4.7%. The results showed that the maximum daily usage of DBB, DBP, and DBHBA was 9.859, 163.445, and 16.399 ng, respectively, which was far below the corresponding permitted daily exposure values according to the safety assessment, indicating that the migration of analytes did not bring any potential safety risk. The compatibility between the drug and the packaging materials was favorable.

CAS / MDL: 84-74-2
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