TALANTA
·
2015
·
IF 3.545
Weibo Chai,Huijuan Wang,Ying Zhang,Guosheng Ding
A facile and sensitive dispersive solid-phase extraction (D-SPE) method for the extraction and enrichment of four representative synthetic colorants prior to high performance liquid chromatography analysis was introduced. As highly efficient adsorbents, polydopamine-coated Fe 3 O 4 nanoparticles (Fe 3 O 4 @PDA NPs) were prepared by a simple and green procedure. Several factors affecting the extraction efficiency, mainly including the polymerization time of dopamine, pH of the sample solution, the amount of adsorbent, extraction time and the desorption conditions, were systematically studied. Under the optimized conditions, the enrichment factors for the four colorants were both higher than 176. The limits of detection (LODs) for the established d-SPE-HPLC method were found to be 0.20–0.25 μg L −1 , which were lower than most chromatographic methods previously reported for synthetic colorant analysis. When used for quantitative analysis, wide linearity ranges (1–500 μg L −1 for amaranth and Ponceau 4R, and 0.80–500 μg L −1 for sunset yellow and allure red) were achieved with good correlation ( R 2 ≥0.9995). The developed method was also successfully applied to the analysis of colorants in beverage samples with satisfactory results, demonstrating its reliability and feasibility in real sample analysis.
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SEPARATION SCIENCE AND TECHNOLOGY
·
2017
·
IF 1.106
Ruiqi Liu,Ye Liu,Chunsheng Cheng,Yaling Yang
A novel method based on ionic liquid enhanced magnetic solid-phase extraction (MSPE) coupled with high-performance liquid chromatography (HPLC) for the separation/analysis of phthalate esters (PAEs) in food samples was established. 1-hexyl-3-methylimidazoliu-hexafluorophosphate ([C6MIM][PF6]) was used to coat oleic acid Fe3O4 nanoparticles with core–shell structures to prepare MSPE agents (Fe3O4@OA@IL). The main parameters affecting the extraction efficiency of PAEs were studied. Under the optimal conditions, the calibration curves were linear in the range of 5–5000 ng mL−1 (R2 = 0.9972–0.9998) of four PAEs. The limit of detections (LODs) and relative standard deviations (RSDs, n = 5) of the method were 1.27–2.95 ng mL−1 and 3.9–5.3%, respectively.
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MICROCHIMICA ACTA
·
2016
·Vol. 183
·期 8
·2467-2472
·
IF 4.831
Yang Yang,Ma Xiaowei,Feng Fan,Dang Xueping,Huang Jianlin,Chen Huaixia
The article describes the synthesis of core-shell magnetic nanoparticles (MNPs) of the type Fe 3 O 4 @MIL-100 (MIL standing for Material Institut Lavoisier), and their application as sorbent for magnetic solid-phase extraction (MSPE) of triclosan. The MNPs were prepared via circular self-assembly of ferric chloride and benzenetricarboxylic acid. The functionalized MNPs were characterized by transmission electron microscopy, FTIR and thermogravimetry. Following extraction, triclosan was eluted with ammoniacal methanol and then submitted to HPLC with UV detection. The amount of magnetic microspheres, sample pH and ionic strength, adsorption time, desorption time, desorption solvent and the volume of the eluent were optimized. Under optimum conditions, the method showed good linearity in the 0.1 to 50 mg·kg −1 triclosan concentration range in toothpaste samples. Other features include (a) intra-day and inter-day relative standard deviations (RSD, for n = 4) of <5.5 %, (b) a 30 μg·kg −1 limit of detection, and (c) extraction recoveries between 90.86 % and 101.1 %. The method was successfully applied to the determination of triclosan in children’s toothpaste.
The article describes the synthesis of core-shell magnetic nanoparticles (MNPs) of the type Fe 3 O 4 @MIL-100, and their application as sorbent for magnetic solid-phase extraction (MSPE) of triclosan.
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Journal of the Iranian Chemical Society
·
2017
·Vol. 14
·期 10
·2087-2096
·
IF 1.407
Zhi Kangkang,Zhang Min,Yang Xin,Zhao Haitian,Dong Aijun,Zhang Hua,Wang Jing
In this paper, a kind of surface molecular imprinting polymers in hydrous solution, with glucose selectively recognition, was successfully synthesized by surface molecular imprinting method, using glucose (Glu) as template molecule, acrylamide as functional monomers, N,N ′-methylenebisacrylamide as the cross-linking agent, ammonium peroxydisulfate as the initiator, activated silica gel (SiO 2 @NH 2 ) as support particles. The influences of cross-linker, initiator as well as support particles amount on the adsorption capacity of Glu-MIPs were performed by single-factor experiments. The optimum conditions were 100 mg of cross-linker, 25 mg of initiator and 1 g of SiO 2 @NH 2 . The adsorption and thermodynamics research revealed that the adsorption of MIPs was fitted to Langmuir, maximum imprinting factor of 2.49 and maximum absorption capacity of 50.06 mg/g. Furthermore, a procedure of extraction of glucose from real fruits samples using the Glu-MIPs as solid-phase extraction adsorbent was developed to apply in analytical techniques.
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TALANTA
·
2017
·
IF 4.162
Dandan Guo,Chaoyan Lou,Nani Wang,Meilan Chen,Peimin Zhang,Shuchao Wu,Yan Zhu
A novel high performance liquid stationary phase was prepared by grafting poly amidoamine (PAMAM) dendrimers to poly (styrene-divinyl benzene-glycidylmethacrylate) matrix in this work. Different generations of PAMAM dendrimers grafted to polymer matrices containing different glycidylmethacrylate amounts by reacting with epoxy groups in glycidylmethacrylate molecules. The synthesized PAMAM dendrimers and stationary phase were characterized by fourier transform infrared spectroscopy, scanning electron microscope, N 2 adsorption/desorption, elemental analysis and thermo gravimetric analyzer. The proposed stationary phase was suitable for rapid separation of phenylene diamine isomers and aminobenzene . The separation mechanism of benzene rings attraction and amino repulsion was verified by retention behaviors of methylamine , phenylamine, phenylene diamine, naphthylamine and toluene. The reliability of the stationary phase was demonstrated by separation and determination of phenylene diamine isomers including m -phenylene diamine, o -phenylene diamine and p -phenylene diamine in hair dye precursors within 10 min. Satisfactory resolution and short analysis time make the columns promising for determination of aniline compounds in various fields.
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TALANTA
·
2016
·
IF 4.035
Jiping Ma,Zhidan Yao,Liwei Hou,Wenhui Lu,Qipeng Yang,Jinhua Li,Lingxin Chen
Magnetic metal-organic frameworks (MOFs, [MIL-101]) were prepared and used as magnetic solid-phase extraction (MSPE) adsorbents for preconcentration of four kinds of pyrazole/pyrrole pesticides (flusilazole, fipronil , chlorfenapyr , and fenpyroximate) in environmental water samples, followed by high-performance liquid chromatography-diode-array detector (HPLC-DAD) determination. Several variables affecting MSPE efficiency were systematically investigated, including amount of MIL-101, extraction time, sample pH, salt concentration, type of desorption solvent and desorption number of times. Under optimized conditions, excellent linearity was achieved in the range of 5.0–200.0 μg/L for flusilazole and fipronil, and 2.0–200.0 μg/L for chlorfenapyr and fenpyroximate, with correlation coefficients r >0.9911. Limits of detection and quantification were 0.3–1.5 μg/L and 1.0–5.0 μg/L, respectively. The intra-day and inter-day precision (relative standard deviation, n =6, %) at three spiked levels were 1.1–5.4% and 3.9–7.8% in terms of peak area, respectively. The method recoveries at three fortified concentration levels ranged from 81.8% to 107.5% for reservoir water samples, 81.0–99.5% for river water samples, and 80.2–106.5% for seawater samples. The developed MOFs based MSPE coupled with HPLC method proved to be a convenient, rapid and eco-friendly alternative to the sensitive determination of pyrazole/pyrrole pesticides with high repeatability and excellent practical applicability.
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MOLECULES
·
2017
·Vol. 22
·期 2
·325
·
IF 2.861
Hong Yao,Bing Chen,Yanyan Zhang,Huigen Ou,Yuxiang Li,Shaoguang Li,Peiying Shi,Xinhua Lin
Selaginella doederleiniiHieron has been traditionally used as a folk antitumor herbal medicine in China. In this paper, the phytochemical components of the total biflavonoids extract fromS. doederleiniiwere studied by using high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry (HPLC-ESI-QTOF MS/MS) in negative ion mode, and their in vitro and in vivo anticancer effects were evaluated. Four types of biflavonoids fromS. doederleinii, including IC3′–IIC8′′, IC3′–IIC6′′, IC3′–IIC3′′′, and C–O linked biflavonoids were examined originally using QTOF MS/MS. The fragmentation behavior of IC3′–IIC3′′′ linked biflavonoids was reported for the first time. A total of twenty biflavonoids were identified or tentatively characterized and eight biflavonoids were found fromS. doederleiniifor the first time. Furthermore, the 3-(4,5-Dimethyl-2-thizolyl)-2,5-diphenyltertazolium bromide (MTT) assay and xenograft model of mouse lewis lung cancer(LLC) in male C57BL/6 mice revealed favorable anticancer properties of the total biflavonoids extracts fromS. doederleinii. The results of this work could provide useful knowledge for the identification of biflavonoids in herbal samples and further insights into the chemopreventive function of this plant.Keywords:Selaginella doederleinii;HPLC-ESI-QTOF MS/MS;biflavonoids;murine B16 melanoma cell;mouse lewis lung cancer (LLC) cell;LLC mouse model
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2025
·
IF 4.6
Lingling Zhao,Xinqi Pan,Jie Shi,Hua Ye,Huanan Guan,Yuanxin Guo,Jian-Jun Zhong
Urocanic acid, like histamine, is a degradation product of histidine that may accumulate over the storage of histidine-rich pelagic fish. Recently evidence from the dermatological and related fields has directed the attention of food scientists toward the adverse health effects of urocanic acid, mostly as a possible “missing factor” responsible for scombrotoxicosis besides histamine. However, experimental effort to study the hypothesis remains scarce, especially regarding the formation of urocanic acid in comparison to the well-documented histamine. Here we report a mixed-mode HPLC method for simultaneously analyzing urocanic acid (both the trans - and cis -isomers), histamine, and histidine in chub mackerel ( Scomber japonicus ) fillets and the use of the method to monitor their changes in concentration at typical refrigeration and abuse temperatures. The method features a simple, reliable chromatographic analysis in cation-exchange/reversed-phase/hydrophilic-interaction triple mode of retention, without the need of precolumn derivatization or addition of ion-pairing agents. At both 4 and 20 °C slow but consistent formation of trans -urocanic acid was observed over time with a relatively faster rate at 20 °C. Histamine formation, by contrast, occurred at 20 °C but ceased completely at 4 °C. In addition, we demonstrate the occurrence of trans -to- cis isomerization of UCA in chub mackerel fillets upon direct sunlight exposure: under our conditions, an isomerization yield around 13 % was achieved within hours on a sunny winter day. Overall, this study provides a chemical analysis method and relevant data for exploring the possible role of urocanic acid in the aetiology of scombrotoxicosis.
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JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Zi-Yu Li,Jia-Hui Zhu,Yu-Zhuo Xu,Jie Zhao,Yu-Shen Liu,Lu-Liang Wang,Shu-Yang Sun,Shi-Lei Ji
Novel magnetic covalent organic frameworks (COFs) were prepared by one-pot synthetic strategy and employed as an efficient adsorbent for magnetic solid-phase extraction (MSPE) of naphthaleneacetic acid (NAA) in food samples. Depending on the predesigned the hydrogen bonding, π-π and hydrophobic interactions of magnetic COFs, the efficient and selective extraction process for NAA was achieved within 15 min. The magnetic COFs adsorbent combined with HPLC-UV was devoted to develop a novel quantitative method for NAA in complex food. The method afforded good coefficient in range of 0.002–10.0 µg mL -1 and low limit of detection was 0.0006 µg mL -1 . And the newly established method afforded less adsorbent consumption, wider linearity and lower LODs than the reported analytical methods. Ultimately, the method was successfully applied to determine NAA in fresh pear, tomato and peach juice. The magnetic COFs based MSPE coupled with HPLC-UV method provided a simple, efficient and dependable alternative to monitor trace NAA in food samples.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2024
·
IF 3.8
Wu Jiaxin,Yao Shunying,Wang Yiwei,Fan Sai,Cui Xia,Chen Dawei,Shi Zhixiong
Organophosphate esters (OPEs) are commonly used chemicals and are also regarded as emerging environmental pollutants. Recently, it has been proved that metabolites of OPEs (mOPEs) could also cause health concerns. However, analytical methods for the concurrent measurement of OPEs and mOPEs in human matrices are still complicated. In this study, a convenient and efficient analytical method combining a cold-induced strategy and HPLC–MS/MS was developed to simultaneously determine 18 OPEs and 10 mOPEs in human serum, urine, and human milk. In brief, after the sample was extracted with acetonitrile, a “one-step” treatment combining purification and enrichment was accomplished by cold-induced liquid–liquid extraction (CI-LLE), and analytes were then quantified by HPLC–ESI–MS/MS. The ratio of acetonitrile/water, and the temperature and time set in the CI-LLE procedure were optimized for achieving the highest enrichment factors. Under the best conditions, linearity, limits of detection (LODs), recovery, precision, and matrix effects of OPEs/mOPEs were verified. LODs of OPEs/mOPEs in serum, urine, and human milk were 0.1–113 pg/mL, 0.1–22 pg/mL, and 0.2–22 pg/mL, respectively. Average recoveries ranged from 80 to 123%, with relative standard deviations lower than 15% for most analytes. The matrix effect test showed slight signal enhancement or inhibition, and the use of isotopically labeled internal standards (ISs) could compensate for the effects. In real sample analysis, both OPEs and mOPEs showed high detecting frequency, which indicated their ubiquity in humans.
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Natural Product Communications
·
2024
·
IF 1.5
Yan Lei,Bing Wang,Guanglin Zhu,Guo Feng,Wei Li,Caiyao Han,Qian Qin,Xie-an Yu,Xueli Song,Zhengyan He,Ju Zhang,Hongmei Su,Wenjing Wang
Background: In the research of the pharmacological activity of modern Chinese medicine, a large number of traditional Chinese medicines show anti-inflammatory activity. Asparagi radix is one of the anti-inflammatory drugs. With the deepening of people's research on Asparagi radix, its anti-inflammatory pharmacological effects have been gradually explored, but its specific anti-inflammatory active ingredients are still unclear. Therefore, it is necessary to screen and identify its specific anti-inflammatory active ingredients from Asparagi radix. At present, COX-2 is an important target for the treatment of chronic inflammation, and many drugs targeting this target have been marketed. However, some drugs have serious side effects, so it is very meaningful to study new COX-2 inhibitors. Methods: In this experiment, the fractions of different time periods are separated by high performance liquid chromatography-separation-trapping system (HPLC-CAD-FC). Then, ultra-high performance liquid chromatography-quadrupole time-of-flight/mass spectrometry (UPLC-Q-TOF/MS) and biological activity analysis techniques are used to identify the chemical composition and in vitro anti-inflammatory activity of each fraction. Finally, the data is integrated to screen out the substances with potential anti-inflammatory activity in Asparagi radix. Results: The results showed that the method established in this experiment can successfully isolate the active components of Asparagi radix, and four saponins with potential anti-inflammatory activity are identified. Conclusion: In summary, the analysis method established in this study can quickly and effectively screen out its anti-inflammatory active substances, and its potential anti-inflammatory active ingredients are mainly steroidal saponins.
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ANALYTICA CHIMICA ACTA
·
2018
·
IF 5.123
Rong Wang,Wenqing Li,Zilin Chen
Polymer monolithic column based on a green deep eutectic solvent (DES) was prepared for in-tube solid phase microextraction of non-steroidal anti-inflammatory drugs (NSAIDs) in aqueous samples. DES composed of choline chloride and itaconic acid was adopted as functional monomer to synthesize a polymeric monolith inside polydopamine-functionalized poly(ether ether ketone) (PEEK) tube. The obtained monolithic column was characterized with fourier transform infrared spectrometry , X-ray photoelectron spectrometer and field emission scanning electron microscope . An online SPME-HPLC method was developed by connecting the PEEK tube to the HPLC system. Parameters including sampling rate, desorption time, sample pH value and sample volume that can affect the performance of this method were investigated. Under the optimized conditions, the proposed SPME-HPLC method showed high extraction efficiency (enrichment factors about 100), good linearity (R ≥ 0.9997) and good reproducibility (relative standard deviation < 4.32%) for determination of three NSAIDs in aqueous solution. The limits of quantification were found to be in a range of 0.05–0.25 ng mL −1 . The SPME-HPLC method was also successfully applied to detect NSAIDs in lake water and human plasma samples.
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危险品化学品经营许可证（带存储）