NEW JOURNAL OF CHEMISTRY
·
2024
·Vol. 48
·期 21
·9702-9708
·
IF 2.7
An-Xu Ma,Cai-Fang Liu,Yu-Lan Zhu,Zong-Hong Luo,Hong-Mei Zhou,Yue Zhang,Bang-Jin Wang,Jun-Hui Zhang,Sheng-Ming Xie,Li-Ming Yuan
In this work, a chiral core–shell microspheres composite, L-his-MIL-53-NH2@SiO2, was prepared through in situ growth and chiral post-modification strategies. The core–shell microspheres were applied as a novel chiral stationary phase for HPLC enantiomeric separation. Various racemates were separated on the L-his-MIL-53-NH2@SiO2 packed column using n-hexane/isopropanol as the mobile phase. The chiral column showed excellent separation efficiency for fourteen chiral compounds, including alcohols, alkanes, esters, phenols, ketones, and organic acids. The influence of injection mass and temperature on the separation performance of the chiral column were investigated. The relative standard deviations (n = 5) of the retention time and peak area by repeated separation of benzoin are 0.28% and 0.63%, respectively. The results show that the L-his-MIL-53-NH2@SiO2 packed column exhibited good reproducibility and stability. In addition, the chiral resolution ability of the L-his-MIL-53-NH2@SiO2 packed column was compared with that of a commercial chiral column (Chiralpak AD-H). The L-his-MIL-53-NH2@SiO2 packed column exhibits unique advantages in chiral separations that can be complementary to the commercial chiral column. It was demonstrated that the chiral core–shell microspheres composite L-his-MIL-53-NH2@SiO2 prepared based on in situ growth and chiral post-modification strategies has great potential for enantiomeric separation by HPLC.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Chun-Ying Xu,Chang-Qing Zhen,Yu-Jing He,Yuan-Yuan Cui,Cheng-Xiong Yang
The abnormal estrogens levels in human body can cause many side effects and diseases, but the quantitative detection of the trace estrogens in complex biological samples still remains great challenge. Here we reported the fabrication of a novel core-shell structured magnetic cyclodextrin microporous organic network (Fe 3 O 4 @CD-MON) for rapid magnetic solid phase extraction (MSPE) of four estrogens in human serum and urine samples prior to HPLC-UV determination. The uniform spherical core-shell Fe 3 O 4 @CD-MONs was successfully regulated by altering the reactive monomers and solvents. The Fe 3 O 4 @CD-MONs owned high specific surface area, good hydrophobicity, large superparamagnetism, and abundant extraction sites for estrogens. Under optimal conditions, the proposed MSPE-HPLC-UV method provided wide linearity range (2.0–400 μg L −1 ), low limits of detection (0.5–1.0 μg L −1 ), large enrichment factors (183–198), less adsorbent consumption (3 mg), short extraction time (3 min), and good stability and reusability (at least 8 cycles). The established method had also been successfully applied to the enrichment and detection of four estrogens in serum and urine samples with a recovery of 88.4–105.1 % and a relative standard deviation of 1.0–5.9 %. This work confirmed the feasibility of solvent and monomer regulation synthesis of Fe 3 O 4 @CD-MON composites, and revealed the great prospects of magnetic CD-MONs for efficient enrichment of trace estrogens in complex biological samples.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Heping Jiao,Ruixiang Bi,Fangli Li,Jingbo Chao,Guimin Zhang,Lihai Zhai,Ligang Hu,Zhenhua Wang,Caifeng Dai,Bing Li
The complex and cumbersome preparation of magnetic covalent organic frameworks (COFs) nanocomposites on a small scale limits their application. Herein, a rapid and easy route was employed for the preparation of magnetic thiourea-based COFs nanocomposites. COFs were coated on Fe 3 O 4 nanoparticles at room temperature without a catalyst within approximately 30 min. This method is suitable for the large-scale preparation of magnetic adsorbent. Using the as-prepared magnetic adsorbent (Fe 3 O 4 @COF-TpTU), we developed a simple, efficient, and sensitive magnetic solid-phase extraction-high performance liquid chromatography-inductively coupled plasma-mass spectrometry (MSPE-HPLC-ICP-MS) for the enrichment and determination of mercury species, including Hg 2+ , methylmercury (MeHg), and ethylmercury (EtHg). The effects of the experimental parameters on the extraction efficiency, including solution pH, adsorption and desorption time, composition and volume of the elution solvent, salinity, coexisting ions, and dissolved organic matter, were comprehensively investigated. Under optimised conditions, the limits of detection in the developed method were 0.56, 0.34, and 0.47 ng L −1 with enrichment factors of 190, 195, and 180-fold for Hg 2+ , MeHg, and EtHg, respectively. The satisfactory spiked recoveries (97.0–103%) in real water samples and high consistency between the certified and determined values in a certified reference material demonstrate the high accuracy and reproducibility of the developed method. The as-proposed method with simple operation, high sensitivity, and excellent anti-matrix interference performance was successfully applied to the enrichment and determination of trace levels of mercury species in the natural samples with complicated matrices, such as underground water, surface water, seawater and biological samples.
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高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Dechang Xie,Yuxuan Wu,Zhuorui Wang,Xiaoguo Ma
Estrogens are emerging environmental contaminants due to their harmful impact on ecological environment and human health. Because estrogens usually exist at very low levels in water environment with complicated matrix, sensitive and accurate determination of trace estrogens in various environmental water samples is a challenging issue. This work developed a new method for simultaneous trace detection of estrogens in aqueous solution by combining multi-template estrogen molecularly imprinted polymers (MIPs) based magnetic solid phase extraction (MSPE) with solidification of floating organic drop (SFO) based dispersive liquid–liquid microextraction (DLLME) and high performance liquid chromatography. The E-MIPs acted as the adsorbent of MSPE for simultaneous selective extraction of multi-estrogens from water. The eluent of MSPE was further concentrated by SFO-DLLME. A series of experiments were performed to optimize the extraction conditions of MSPE and DLLME, and the obtained results were as follows: solution pH 8.0, 1.5 mL of MeOH/HAc (9:1, v:v) as the eluent, 50 μL of 1-dodecanol as the extractant, extraction for 5 min and using 3 % NaCl. Under the optimum conditions, the detection limits for the selected estrogens were 0.29–1.11 μg L −1 , which were comparable with or even lower than those achieved by using HPLC-MS/MS. The recoveries of estrogens were 90.5–107.0 % in the determination of various environment water samples with RSDs of 1.5–7.0 %. Therefore, the proposed multi-template MIPs-MSPE-DLLME-HPLC method is selective, sensitive, accurate, rapid and without the need of very expensive instrument, which offers a practical approach for the simultaneous trace analysis of estrogens in water.
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FOOD CHEMISTRY
·
2017
·
IF 4.529
Lu Zhang,Zong-cai Tu,Xing Xie,Hui Wang,Hao Wang,Zhen-xing Wang,Xiao-mei Sha,Yu Lu
Jackfruit ( Artocarpus heterophyllus Lam.) peel is an underutilized by-product in both, the production and processing of jackfruit . This research compared the antioxidant and hypoglycemic potential of jackfruit peel with jackfruit pulp, flake and seed for the first time. The phytochemical profile of peel extract was characterized with HPLC-QTOF-MS/MS. Results revealed that peel extract exhibited the highest total phenolic and total flavonoid content, and the phenolics was 4.65, 4.12 and 4.95 times higher than that of pulp, flake and seed extract, respectively. The strongest DPPH and ABTS + scavenging ability, α -glucosidase inhibition were also found in peel extract, and the α -glucosidase inhibition was about 11.8-fold of that of acarbose. The HPLC-QTOF-MS/MS analysis led to the tentative identification of 53 compounds, prenylflavonoids, hydroxycinnamic acids and glycosides are the predominant bioactive compounds. Above results reveal promising potential of jackfruit peel as a new source of natural antioxidants and hypoglycemic agents.
研究领域:
食品科学
·
植物化学
·
药理学
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高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 10
·4091-4098
·
IF 4.58
Liu Haochi,Chen Ligang,Ding Jie
The authors describe an efficient method for the extraction of tetracycline antibiotics (TCs) from water samples by using a new kind of core-shell adsorbent. It consists of a magnetite (Fe 3 O 4 ) core and a metal-organic framework (type ZIF-8) as the shell. The sorbent has a large specific surface and superparamagnetic response. The sorbent was characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, nitrogen adsorption, and X-ray diffraction. The adsorption isotherms, dynamic adsorption, and mechanisms of interactions between tetracycline and sorbent were studied. Various parameters affecting the extraction efficiency were optimized. Following desorption of the TCs with methanol (containing 1% of acetic acid), they were quantified by using ultra-high performance liquid chromatography combined with mass spectrometry. The method has a linear range that extends from 0.5 to 50 ng·L −1 , and the limits of detection for tetracycline, chlortetracycline, and oxytetracycline are 0.125, 0.122 and 0.143 ng·L −1 , respectively. The relative standard deviations of intra-day and inter-day assays range from 3.3% to 8.5%, and from 2.8% to 8.3%, respectively. The recoveries of TCs (at spiking levels of 0.5, 5.0 and 50 ng·L −1 ) are in the range between 78.3% and 93.7%. The method was successfully applied to the determination of TCs in spiked river water, fish pond water, and livestock wastewater.
研究领域:
环境科学
·
分析化学
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高影响因子
CHROMATOGRAPHIA
·
2013
·Vol. 76
·期 13
·735-745
·
IF 1.437
Peng Xi-Tian,Li Ze,Zhang Yi,Liu Tao,Yu Qiong-Wei,Feng Yu-Qi
A novel mixed-mode stationary phase (OAS) has been prepared by bonding n -octyl and aminopropyl groups with the surface of silica gel. The obtained OAS stationary phase was characterized by Fourier transform infrared spectroscopy, elemental analysis, zeta potential and ion-exchange capacity. The mixed-mode one-site and two-site retention models were used to quantitatively describe the retention mechanism of the OAS stationary phase using three strong acidic analytes. The results indicated that the two-site model is more suitable for the description of mechanism of OAS phase. Then the OAS stationary phase was applied to separate ten water- and fat-soluble vitamins in a single run; the separation is based on the hydrophobic and ionic interaction mechanisms. A method for the simultaneous determination of ten water- and fat-soluble vitamins in commercial multivitamin tablets by high performance liquid chromatography with ultraviolet detection was established and validated according to the stability, linearity, accuracy and precision. Finally, the validated method was used to analyze the content of ten vitamins in two commercial multivitamin tablets and the recoveries were in the range of 89.2–111.0 %, with RSDs <6.1 %, indicating the good reliability of the proposed method.
研究领域:
分析化学
·
药物分析
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JOURNAL OF SEPARATION SCIENCE
·
2015
·Vol. 38
·期 21
·3774-3780
·
IF 2.737
Fuyou Du,Xian Zheng,Lin Sun,Qun Qin,Lin Guo,Guihua Ruan
A polymerized high internal phase emulsion monolith was used as a novel sorbent for solid-phase extraction coupled with high-performance liquid chromatography and fluorescence detection for the determination of oxytetracycline, tetracycline, doxycycline, and chlorotetracycline in environmental water samples. The polymerized high internal phase emulsion monolithic column was prepared by the in situ polymerization of the continuous phase of a high internal phase emulsion containing glycidyl methacrylate, styrene, and divinylbenzene in pipette tips, and then functionalized with iminodiacetic acid. The resulting monolith exhibited highly interconnected porosity and large surface areas, making it an excellent candidate as an solid-phase extraction sorbent for the enrichment of trace tetracycline antibiotics. Several factors affecting the extraction performance of polymerized high internal phase emulsion monoliths, including the pH of sample solution, the eluting solvents, the sample loading flow rate and volume, were investigated, respectively. Under the optimized conditions, the mean recoveries of oxytetracycline, tetracycline, doxycycline, and chlorotetracycline spiked in pond and farm wastewater samples ranged from 78.1 to 119.3% with relative standard deviation less than 15%. The detection limits (S/N = 3) of the proposed method were in the range of 51–137 pg/mL. This study demonstrated that the monolithic polymerized high internal phase emulsion would be promising solid-phase extraction sorbents in the extraction and proconcentration of trace analytes from complex samples.
研究领域:
分析化学
·
环境科学
·
药物残留检测
·
色谱技术
·
样品前处理
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高影响因子
TALANTA
·
2016
·
IF 4.035
Lijie Liu,Lian Xia,Chuanxiang Wu,Fengli Qu,Guoliang Li,Zhiwei Sun,Jinmao You
A stable zirconium (Ⅳ)-based metal organic frameworks (UIO-67) material possessing good chemical, thermal and water stability was synthesized and applied as a sorbent for the dispersive solid phase extraction (DSPE) of 8 plant growth regulators (PGRs) in fruit samples. Fluorescence labeling combined with high performance liquid chromatography fluorescence detection (HPLC-FLD), was used to quantify the target analytes. Characterization of the UIO-67 material was performed by X-ray diffraction(XRD) and scanning electron microscopy (SEM). The experimental parameters, such as amount of UIO-67, type and volume of eluting solvent, adsorption and desorption time, were optimized. Under the optimized conditions, good linearity was observed in the range of 10–1000 pmol/mL with R 2 >0.9989. The limits of detection and limits of quantification were in the range of 0.21–0.57 ng/mL and 0.81–1.91 ng/mL, respectively. The intra-day and inter-day precisions (based on the relative standard deviation, n =3) of the PGR derivatives were under 3.1% and 5.3% respectively and the accuracies of the method for the PGRs were in the range from 89.3% to 102.3%. The developed method was successfully applied to analyze PGRs residues in fruit samples. The proposed method is proved to be simple, environment-friendly and inexpensive and it is feasible to directly use UIO-67 as sorbent to extract targets by varying conditions.
研究领域:
分析化学
·
食品科学
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高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2026
·
IF 4.6
Qi Huang,Xiaoqiang Xiang,Wenqing Li,Qinggui Lei,Weiqi Yang,Dan Tang,Zhengming Qian
This study developed a rapid and eco-friendly HPLC method for simultaneous determination of adenosine and ergothioneine in Cordyceps spp. samples. The extracted protocol involved dispersing samples in diatomaceous earth followed by vortex extraction with 80 % methanol. Chromatographic separation was achieved within 5 min using a Shim-pack Velox HILIC column with a gradient mobile phase of 0.1 % formic acid aqueous solution and acetonitrile solution containing 0.1 % formic acid and detection at 260 nm. Both analytes demonstrated excellent linearity ( r > 0.9999) with average recoveries of 102.82 % (adenosine) and 100.10 % (ergothioneine), accompanied by RSD s below 2 %. The contents of adenosine and ergothioneine in 46 batches of Cordyceps spp. samples were 0.000–2.700 mg/g dry weight (DW) and 0.000–0.703 mg/g DW, respectively. The Ophiocordyceps sinensis and its related species were successfully classified by hierarchical cluster analysis. This study determined the content of ergothioneine in Cordyceps spp. samples for the first time, and identifies ergothioneine as a critical marker for differentiating authenticated Ophiocordyceps sinensis from its adulterants. Results of BAGI assessment (score=87.5) confirmed the superior practicality and environmental friendliness of the developed method. This rapid, accurate, and reliable method provided a scientific foundation for enhancing quality evaluation technology of Cordyceps spp. species samples.
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Food Analytical Methods
·
2026
·Vol. 19
·期 1
·60
·
IF 3
Hussain Aisha,Wu Jiapeng,Wen Jiaxi,Xiong Chaomei
Sudan dyes, a class of azo dyes, are genotoxic and carcinogenic to humans. However, they are still used illegally to color food products and spices due to their color fastness. In this study, multi-functionalized magnetic silica nanoparticles (C 18 /DVB/NVP(4:1)-Fe 3 O 4 @SiO 2 MNPs) were synthesized, and solid–liquid extraction (SLE) coupled with magnetic solid phase extraction (MSPE) was employed for the extraction and preconcentration of five Sudan dyes (Sudan I − IV, Sudan Red 7B), followed by high-performance liquid chromatography/ultraviolet spectroscopy (HPLC–UV) for their detection in powdered chili pepper samples. The SLE conditions for the analytes in powdered chili pepper samples were optimized. Under optimal conditions, the extraction recovery ranged between 78.0% and 106.9%. We investigated and optimized the potential factors that may affect the efficiency of MSPE. Under these optimal conditions, calibration curves showed good linearity ( R 2 > 0.9989) across the tested concentration range of 0.98 to 125 µg/g. The limits of detection for the five Sudan dyes were in the range of 0.06–0.26 µg/g. The intra-day and inter-day accuracy ranged from 93.5% to 106.3% with a relative standard deviation (RSD) of not more than 9.1%. The developed method was successfully applied to analyze ten different commercial brands of powdered chili pepper samples purchased from markets in Wuhan, confirming its feasibility for routine analysis of illegal Sudan dyes in these samples.
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MOLECULES
·
2026
·Vol. 31
·期 12
·2138
·
IF 5.1
Xiaoduo Ma,Lei Xing,Ranran Feng,Shumin Hu,Wei Yong,Tianyang Guo,Zhaoxia Yang,Huanlu Song
Whisky is well-known worldwide owing to its unique flavor, and its fermentation and distillation conditions have a significant effect on its aroma. In this paper, new-make spirits were prepared by four fermentation conditions (two distilling yeasts and two fermentation temperatures), and the different stages (wort, wash, low wine, and new-make spirit) of the samples were collected. The main aroma compounds and their precursors were initially determined in wort and wash samples by GC-MS, UPLC-MS and HPLC. Results showed that Strecker degradation, reduction, and esterification occurred during the fermentation process, leading to decreased contents of amino acids and increased contents of volatile esters, alcohols, and acids. Moreover, the two distilling yeasts exhibited their respective optimal fermentation temperatures. Then, the distillation process was evaluated by two-dimensional gas chromatography–olfactory–mass spectrometry (GC×GC-O-MS), and 74 aroma compounds were found in different stages of new-make whiskies fermented by the two distilling yeasts and one brewer’s yeast. The contents of most compounds were enhanced by at least ten times after two distillations, while the contents of some sulfur compounds decreased. Finally, the feature aroma-active compounds of each new-make whisky were identified according to rOAV. These results provided theoretical and methodological support for yeast selection and process control in whisky production.
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高影响因子
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