JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2012
·Vol. 50
·期 7
·620-624
·
IF 0.884
Xie Kaizhou,Jia Longfei,Xu Dong,Guo Huisheng,Xie Xing,Huang Yuping,Chen Xuesen,Bao Wenbin,Dai Guojun,Wang Jinyu
A sensitive and robust method is presented for the simultaneous determination of amoxicillin (AMO) and ampicillin (AMP) in eggs by reversed-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC–FLD). This method used a simple liquid–liquid extraction of the samples with acetonitrile and dichloromethane as precipitation of proteins and extraction solvent. AMO and AMP reacted with salicylaldehyde to form fluorescent derivatives, which were then analyzed with RP-HPLC–FLD. Separation was carried out on an Athena C18 column with a mobile phase consisting of 0.01M potassium dihydrogen phosphate, adjusted to pH 5.5 by 2M potassium hydroxide and acetonitrile. The detector response was linear over the tested concentration range from 5.0 to 800 ng/mL for AMO and AMP. The recovery values ranged from 78.4 to 88.7% for AMO and from 77.6 to 82.0% for AMP. The limits of detection were 1.2 for AMO and 0.4 µg/kg for AMP. The limits of quantification were 3.9 for AMO and 1.5 µg/kg for AMP. The corresponding intra-day and inter-day variation (relative standard deviation) were found to be less than 9.6 and 14.8%, respectively.
研究领域:
分析化学
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食品科学
·
药物分析
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DOI
PubMed
高影响因子
KEY ENGINEERING MATERIALS
·
2017
·
IF 0
Xi De Xu,Jie Liu,You Ping Wu,Jian Ping Deng
Novel biocompatible tough hydrogels were prepared through free radical micellar polymerization of N-isopropylacrylamide (NIPAM) with ammonium persulphate (APS) as initiator, in which hydrophobic monomer stearyl acrylate (C18) underwent micellar polymerization in the presence of gelatin as emulsifier. FT-IR and DSC demonstrated the formation of co-polymer of NIPAM and C18. Swelling results indicated that hydrophobic polymer domains derived from C18 in aqueous medium acted as the physical crosslinking points by hydrophobic association. Uniaxial tensile test demonstrated the mechanical properties of hydrogels increased with increasing C18 and gelatin contents. The hydrogel exhibited low toxicity and promoted cell proliferation. The desirable toughness, low toxicity and the promoting effect of cell proliferation made the present hydrogels good candidates for tissue regeneration materials.
研究领域:
材料科学
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生物材料
·
组织工程
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产品关联
DOI
Toxins
·
2025
·Vol. 17
·期 9
·445
·
IF 4
Bo Zhang,Yang Liu,Shengnan Li,Ruonan Li,Yunhui Zhang,Hua Zhao
Wild mushroom poisoning is an emerging global food safety issue, especially in subtropical regions like southwestern China, where incidents are geographically clustered. Current detection methods are often time-consuming and overlook region-specific toxins. We developed a rapid, sensitive, and accurate method for the simultaneous detection of ten characteristic mushroom toxins prevalent in Guizhou, China. The method combines graphite multi-walled carbon nanotubes (G-MWCNTs) for sample preparation with Orbitrap high-resolution mass spectrometry (HRMS). Wild mushroom samples were extracted via ultrasonic-assisted methanol–water extraction, purified using G-MWCNTs, and separated on a Hypersil GOLD C18 column (100 mm × 2.1 mm, 1.9 μm). Gradient elution was performed with 0.1% formic acid + 0.01% ammonia and acetonitrile; quantification used the external standard method. The method achieved LODs of 0.005–0.2 mg/kg and LOQs of 0.015–0.6 mg/kg, with RSDs below 18.11% and excellent linearity (R2= 0.9936–0.9989). Among 45 wild mushroom samples, toxin levels ranged from 0.032 to 445.10 mg/kg, with a detection rate of 22.22%, suggesting notable poisoning risk. This method reduces pretreatment time while ensuring high analytical performance, offering a reliable tool for rapid toxin screening and supporting regional surveillance of wild mushroom poisoning.
研究领域:
分析化学
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食品安全
·
毒理学
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环境监测
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质谱分析
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2014
·Vol. 182
·期 3
·855-862
·
IF 3.719
Yan Fufeng,Zhang Yuanchang,Zhang Shuai,Zhao Jihong,Liu Shunli,He Linghao,Feng Xiaozhong,Zhang Hongzhong,Zhang Zhihong
We report on an efficient method for the production carboxy-modified graphene (carboxy-GR), and its application to a highly sensitive immunoassay for the livestock feed additive clenbuterol. Octadecanoic acid is shown to self-assemble on carboxy-GR via intermolecular interaction. Goat anti-mouse IgG was conjugated to 1-octadecanethiol-modified carboxy-GR and then deposited by self-assembly on a C18-modified gold surface. The resulting sensor surface was used to quantify clenbuterol by both surface plasmon resonance and electrochemical impedance spectroscopy. The assay works in the 0.01 ng∙mL −1 to 10 ng∙mL −1 concentration range and the lower detection limit is 6.57 pg∙mL −1 . It is concluded that this fairly simple method can be extended to immunoassays for other food additives.
Principle of sensor system and immunoassay. (i) Binding of ACG–IgG with the alkyl chain of 1-octadecanethiol through intermolecular force onto the gold substrate; (ii) absorbance of Ab CLB onto the surface of ACG-IgG; and (iii) detection of CLB using an immunoassay based on Ab CLB –ACG–IgG.
研究领域:
材料科学
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分析化学
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食品安全
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生物化学
·
纳米技术
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产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 13
·2161-2176
·
IF 3.614
Yan-lin Zhao,Lin-lin Zhao,Yu-xin you,Xiao-xiao Zheng,Yan Du,Dao-quan Tang
We aim to establish a simple and easy high-performance liquid chromatography system coupled with an ultraviolet detector suitable for simultaneous determination of 24 antiepileptic drugs in human plasma. Optimized chromatographic separation was performed on a ZORBAX Eclipse Plus-C18 (4.6 × 150 mm 2 , 3.5 μm) column with acetonitrile and 5 mM potassium dihydrogen phosphate water solution as mobile phase. Note that, 24 antiepileptic drugs were divided into three groups and eluted with different gradient procedures, respectively. The column temperature was maintained at 35°C and the detection wavelength was set at 210 nm. Plasma was processed with ethyl acetate or acetonitrile. The calibration curves of 24 antiepileptic drugs demonstrated good linearity within the test range ( r > 0.996). The intra- and inter-batch precision and accuracy were all less than 15%, while extraction recoveries were in the range of 74.57–90.89% with the relative standard deviation values less than 15%. The validated methods have been successfully applied to determination of some antiepileptic drugs in rat or patient plasma. Those results indicated that the developed methods were simple and easy, and could be suitable for the determination of 24 antiepileptic drugs in plasma just by changing the gradient elution procedures of mobile phase.
研究领域:
分析化学
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药理学
·
临床化学
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DOI
高影响因子
RSC Advances
·
2018
·Vol. 8
·期 29
·15906-15914
·
IF 2.936
Zhaokun Yan,Qingtang Wang,Xiaolong Liu,Jun Peng,Qin Li,Ming Wu,Jiumao Lin
Ursolic acid (UA) has shown great potential in cancer therapy but their efficacy is seriously compromised by poor water-solubility and limited cellular uptake. In this paper, cationic nanomicelles self-assembled from Pluronic F127 with the cationic polymer of C18-polyethylenimine (C18-PEI) as a functional component are fabricated as delivery vehicles of Chinese herbal medicine active components of ursolic acid (UA) for colorectal cancer treatment. The inhibition effects of this drug loaded cationic nanomicelles (named as FUP) on cell viability and cell colony formation were more significant than the free UA, due to their cationic surface which can increase UA uptake by colorectal cancer cells. Cell cycle analysis showed that this inhibition effect was mediated by a cell cycle arrest at the G1 checkpoint, and the cell death induced by these nanomicelles occurred via apoptosis, which was detected by annexin V antibody and propidium iodide staining. Further western blot analysis demonstrated the apoptosis mechanism was associated with the regulation of Fas/FasL and activation of caspase-8 and caspase-3. Therefore, our cationic nanomicelles can potentially be used to enhance the therapeutic effect of UA for colorectal cancer treatment.
研究领域:
药学
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纳米技术
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肿瘤学
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中药
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DOI
PubMed
高影响因子
Journal of Inorganic and Organometallic Polymers and Materials
·
2019
·Vol. 30
·期 3
·859-868
·
IF 1.637
Cheng Lingping,Cai Jianfeng,Ke Yanxiong
Core–shell particles (CSPs), also known as superficially porous particles or fused-core particles, consisting of a solid core and a porous shell, have emerged as an advanced technology in high-performance liquid chromatography (HPLC). We report here an ultrasonic-assisted sol–gel method for the fabrication of CSPs with uniform mesoporous silica shell using tetraethoxysilane as the silica source and dodecylamine as a catalyst, template and porogen agent in a methanol–water solution. Instead of stirring, sonication was adopted to guarantee the particles monodispersity and uniformity. The shell thickness between 300 and 700 nm could be obtained by adjusting the sonication time and the volume ratio of methanol–water. Pore sizes from 3.4 to 8.5 nm were tuned by hydrothermal treatment. The C18-bonded 2.7 μm CSPs with a shell thickness of ~ 500 nm showed some advantages over a commercial 1.7 μm BEH column, and successfully applied for the analyses of a Chinese medicine and peptides. The CSPs could be a promising candidate as HPLC packing materials.
研究领域:
分析化学
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材料科学
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纳米技术
·
药物分析
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产品关联
DOI
高影响因子
Heliyon
·
2023
·
IF 4
Hengyi Yu,Dongyan Li,Dong Xiang,Xiping Li,Lu Liu,Dong Liu,Xuepeng Gong
A rapid, specific and accurate high-performance liquid chromatography with tunable ultraviolet detection method was developed to simultaneously determine azathioprine metabolites, 6-thioguanine nucleotides (6-TGN) and 6-methyl mercaptopurine riboside (6-MMPr) in human red blood cells. Erythrocyte lysate sample was precipitated by perchloric acid under the protection of dithiothreitol, with 6-TGN and 6-MMPr being acid hydrolyzed to produce 6-thioguanine (6-TG) and 6-methymercaptopurine (6-MMP). A Waters Cortecs C 18 column (2.1 × 150 mm, 2.7 μm) was used for chromatographic separation with a water (containing 0.01 mol/L ammonium acetate and 0.2% acetic acid)/methanol linear gradient at a flow rate of 0.45 mL/min in a 5.5 min. UV detection wavelengths were 340 nm for 6-TG, 303 nm for 6-MMP and the IS (5-bromouracil). The calibration curves fitted a least squares model (weighed 1/ x 2 ) from 0.15 to 15 μmol/L for 6-TG ( r 2 = 0.9999) and from 1 to 100 μmol/L for 6-MMP ( r 2 = 0.9998). This method was validated according to the FDA bioanalytical method validation guidance and ICH M10 bioanalytical method validation and study sample analysis guidance for industry, and successfully utilized in ten IBD patients receiving azathioprine therapy.
研究领域:
药理学
·
分析化学
·
临床化学
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DOI
PubMed
高影响因子
RSC Advances
·
2024
·Vol. 14
·期 46
·34261-34269
·
IF 3.9
Min Xie,Jun Xu,Dan Fei,Ye-Lan Guang,Yao-Min Zhou,Fan Li,Li-Zhen Hu
An improved QuEChERS method combined with Multi-Plug Filtration Cleanup (m-PFC) clean-up procedure was developed for the simultaneous determination of 16 different sulfonamides in forage grasses using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The forage grass sample was extracted with 0.1 mol L−1 Na2EDTA-Mcllvaine buffer and acetonitrile solution, purified by the Navo U-QuE column tube, separated by Agilent ZORBAX Eclipse Plus C18 column, and analyzed by MRM (multiple reaction monitoring) mode and the internal standard method was utilized for quantification. The 16 different sulfonamides display good linearity within the range of 0.5–50 μg L−1 (R2 > 0.9967), the limit of detection was 0.02–0.5 μg kg−1, and the limit of quantification was 0.05–1.0 μg kg−1. Under the additive amounts of 1, 2, and 10 μg kg−1, the recoveries were in the range of 72.3–116.9%, and the relative standard deviation was between 1.4% and 10.3%. The presented method showed the advantages of simple operation, excellent selectivity and high sensitivity. It was well-suited for both qualitative and quantitative analyses of sulfonamides in forage grass. Overall, this method provided a scientific basis for risk assessment, enforcement of quality and safety standards, and detection of sulfonamide residues in forage grass for import and export.
研究领域:
分析化学
·
兽医学
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食品安全
·
药物分析
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Yanyan Wang,Liuqian Bao,Jiajing Sun,Yuanyuan Ding,Jiasheng Shi,Zhengyu Duan,Zhiyong Chen
Fluorous affinity chromatography has received growing attention in separation and purification of fluoro compounds, but the wettability of the fluorinated stationary phases is seldom noticed. Here, we construct a series of micro-sized fluorine-containing microspheres by solvothermal precipitation polymerization. The fluorinated microspheres could be obtained with narrow size distribution at even high monomer loading of 15 wt%. Through alternating fluoro monomer, both the particle size and the wettability of the microsphere array could be tuned. Among them, the poly(divinylbenzene -dodecafluoroheptyl methacrylate), P(DVB-DFHMA), microsphere (6.1 μm) arrays displays superhydrophobicity with 153.2° water contact angle. The P(DVB-DFHMA) fluorinated microspheres (7.58% fluorine content) can be packed into steel-less columns as stationary phase for high-performance liquid chromatography. The retention mechanism of the fluorinated column is proven to be the specific fluorine-fluorine interaction. Compared to the commercial C18 silica column, the fluorinated column can completely separate fluorine-containing compounds under high water content mobile phase, including small fluoro molecules and fluoro macromolecules, at much lower back pressure by fluorous affinity.
研究领域:
化学
·
材料科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Zhefei Hu,Yanhao Jiang,Panpan Cao,Yanjuan Liu,Yuefei Zhang,Wei Chen,Sheng Tang
In this work, 2-undecylimidazole (UI) and propyl methacrylate (PMA) dual-functionalized silica gel was prepared and applied as a mixed-mode chromatographic stationary phase. Successful preparation of this stationary phase (SiO 2 -UI-PMA) was proved through a range of characterization techniques. The chromatographic performance of the obtained SiO 2 -UI-PMA was investigated for the separation of environmental endocrine disruptors (phthalates, steroid hormones, bisphenols and alkylphenols), sulfonamides and food-borne stimulants in reversed-phase chromatography, as well as for the separation of inorganic anions in anion-exchange chromatography. The effect of column temperature, acetonitrile content, salt concentration and mobile phase pH on retention was studied to explore the separation mechanism, and the results indicated that this stationary phase provided multiple interactions with analytes. Compared with the commercial C18 column, the SiO 2 -UI-PMA demonstrated more preferable separation ability under the mobile phase conditions with a low content of acetonitrile, thereby acting as a good alternative candidate for the conventional reversed-phase stationary phase in chromatographic analysis. Furthermore, the SiO 2 -UI-PMA stationary phase exhibited high column efficiency (45 860 plates m −1 for progesterone) even though it was prepared from the non-serviceable silica based chromatographic packing materials.
研究领域:
分析化学
·
环境科学
·
材料科学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Kaiqi Yan,Xiangwei Liu,Jiawei Liu,Chong He,Jian Li,Quan Bai
A high-throughput sample pre-treatment method combined with high-performance liquid chromatography (HPLC) was developed to analyze phthalates (PAEs) in food and food contact package samples. Thin film microextraction (TFME) in 96-blade format was used to pre-treat 96 samples simultaneously. Octadecyl groups functionalized fibrous mesoporous silica nanospheres, namely C18-FMSNs, were synthesized and used as TFME coating material. The coating was fabricated by spraying a slurry of C18-FMSNs and polyacrylontrile (PAN) mixture with a commercial portable spraypen. The prepared C18-FMSNs/PAN coatings exhibited good reproducibility, repeatability and reusability. The optimized TFME conditions for PAEs consisted of extraction at pH 4.0 for 50 min, and desorption by methanol/acetonitrile (25/75, V/V) for 40 min. The pretreatment time for each sample was approximately 1.3 min. This TFME-HPLC method showed good linearity for eight PAEs within the concentration range of 0.5–1000 ng mL −1 , with the coefficients higher than 0.9972. The limits of detection and quantification were 0.096–0.26 ng mL −1 and 0.32–0.86 ng mL −1 , respectively. The intra-day and inter-day RSD % were below 6.6 % and 8.4 %, respectively, indicating good precision. The PAEs analysis in real samples showed that dibutyl phthalate (DBP) of 2.3 ± 0.3 ng mL −1 and di-(2-ethylhexyl) phthalate (DEHP) of 5.5 ± 0.8 ng mL −1 in boxed milk, dimethyl phthalate (DMP) of 12.6 ± 0.8 ng mL −1 , DBP of 3.2 ± 0.4 ng mL −1 and DEHP of 14.3 ± 0.7 ng mL −1 in the simulated water migration of plastic box, as well as DMP of 19.0 ± 0.6 ng mL −1 , DBP of 25.6 ± 0.9 ng mL −1 and DEHP of 49.5 ± 2.8 ng mL −1 in the simulated ethanol migration of plastic box were determined, respectively. In addition, the detection of PAEs in all the real samples showed good recovery ranging from 85.6 to 110 % and lower RSDs % (<7.2 %).
研究领域:
分析化学
·
食品科学
·
材料科学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）