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CHEMICAL RESEARCH IN CHINESE UNIVERSITIES · 2018 ·Vol. 34 ·期 4 ·665-669 · IF 1.248

Study on the Preparation of Mercaptoacetic Acid-modified Heterophylla Shell and Its Application in Separation and Enrichment of Pb2+ in Environmental Samples

Lyu Linlin,Jiang Xiaojun,Jia Lian,Ai Tian,Wu Hang

To increase the adsorption capacity of the Corylus heterophylla Fisch(HS) for Pb 2+ , HS was chemically modified using NaOH aqueous solution and 95% ethanol and was labeled as SHS; then SHS was chemically modified using mercaptoacetic acid. The SHS modified with mercaptoacetic acid(MHS) was characterized using FTIR, SEM, and XPS. The results indicated that the —SH group was present on MHS, and after Pb 2+ adsorption, the absorption value of the characteristic peak of the —SH group decreased. The adsorption and desorption properties of this functionalized material were investigated as well as the influences of parameters, such as pH value, type of desorption reagent, dosage, flow rate and maximum sample volume. The Pb 2+ adsorption of MHS reached a maximum with pH>5. The experimental data of Pb 2+ adsorption using MHS were fitted using the Langmuir isothermal adsorption model, and a maximum adsorption capacity of 61.54 mg/g was obtained. This was much higher than the adsorption capacity of SHS before modification with the thiol group. After adsorption, MHS was desorbed using a 0.2 mol/L HCl solution, and the percent of desorption was higher than 99%. MHS was used as a solid-phase extractant in the analysis and determination of Pb 2+ content in food and water samples, and the enrichment times achieved 150-fold.

研究领域: 环境科学 · 材料科学
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2025 · IF 3.8

Alkanol–hexafluoroisopropanol high-density supramolecular solvent-based dispersive liquid–liquid microextraction of antipsychotics in human urine

Li Xiao,Chen Jia,Li Xuanwei,Xia Yaokun,Zhao Qingwei

A dispersive liquid–liquid microextraction method based on high-density alkanol–hexafluoroisopropanol supramolecular solvent (alkanol–HFIP SUPRAS) coupled with liquid chromatography-tandem mass spectrometry is presented for microextraction and detection of four antipsychotics (aripiprazole, lurasidone, risperidone, and paliperidone) in urinary specimens. With octanol as the extractant and HFIP as the dispersant, SUPRAS-forming agent, and density regulator, reverse micelle aggregate-based SUPRAS spontaneously formed in urine, which acted as SUPRAS inducer and analytical sample. SUPRAS formation was not limited by sample pH or salt addition. The SUPRAS, located at the bottom layer of the sample solution due to its high density, was easily collected in trace volumes (~14 μL). Extraction conditions were studied and screened by the one-variable-at-a-time method, the Box–Behnken design, and response surface modeling. Optimal conditions provided low solvent consumption (70 μL of octanol and HFIP), short extraction time (40 s of vortex time), high extraction rate (61–78%), and good enrichment factor (44–55). There is a good linear relationship with correlation coefficients higher than 0.9959. Method limits of detection (S/N = 3) and quantification (S/N = 10) were in the ranges of 0.13–0.38 ng mL −1 and 0.42–1.28 ng mL −1 , respectively. Recoveries ranged from 94.0 to 120.3% with intra- and inter-day relative standard deviations less than 9.9%. The method also has satisfactory levels of eco-friendliness and sustainability (0.56 of AGREEprep score) with low matrix effects (87.4–113.0%). The method is a fast, simple, efficient, and environmentally benign procedure for microextraction and detection of antipsychotics in human urine.

CAS / MDL: 915-67-3
研究领域: 分析化学 · 药物分析 · 临床化学 · 环境化学
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MICROCHIMICA ACTA · 2025 ·Vol. 192 ·期 8 ·1-12 · IF 5.3

Highly stable benzonitrile functionalized covalent organic framework coating for solid-phase microextraction of hydroxyphenyl esters in complex matrix samples

Dong Zong-Mu,Qin Liming,Guo Yaqing,Xu Miaoqing,Wu Jian-Feng,Zhao Guang-Chao

A mesoporous surface benzonitrile functionalized covalent organic framework (TpBD-CN-COF) was synthesized as a novel solid-phase microextraction (SPME) fiber coating for the extraction of six hydroxyphenyl esters (PBs), and combined with gas chromatography-flame electric-ion detector (GC-FID). PBs were sensitively determined in aqueous solution. Due to its high specific surface area, high chemical stability in both strongly acidic and alkaline media, and in polar or non-polar media, as well as its high thermal stability, the TpBD-CN-COF fiber coating showed excellent extraction performances for PBs with an enrichment factor twice as high as that of TpBD-COF. Some parameters that influenced the extraction performance, such as extraction time and temperature, pH, and stirring speed were investigated. Under optimal conditions, a wide linear range (0.06–500 μg L −1 ), low limits of detection (LOD, 0.003–0.042 μg L −1 ) were obtained for PBs determination. The relative standard deviations (RSDs, n  = 6) for intra-day, inter-day, and fiber-to-fiber were less than 8.06%, 7.8%, and 8.6%, respectively. Furthermore, the analytical method could be successfully used to detect six PBs in cosmetics and environmental water samples, achieving satisfactory recoveries ranging from 85.14 to 107.67%. Graphical

研究领域: 分析化学 · 材料科学 · 环境化学 · 分离科学 · 化学分析
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