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Preparation of Molecularly Imprinted Composites Initiated by Hemin/Graphene Hybrid Nanosheets and Its Application in Detection of Sulfamethoxazole

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Current Medical Science 2019年第1期39卷 159-165页

作者： Shao-fei GUO Xiao-yu CHEN Peng WANG Cheng CHEN Rui-hua PAN Yue-tao LING Yi-zhu TANG hubei entry-exit inspection and quarantine bureau of prc Wuhan 430022China hubei Institute of Sport Science Wuhan 430205China

Molecularly imprinted polymers(MIPs)exhibit high selectivity resulting from imprinted cavities and superior performance from functional materials,which have attracted much attention in many ***,the combination of MIPs film and functional materials is a great *** this study,hemin/graphene hybrid nanosheets(H-GNs)were used to initiate the imprinted polymerization by catalyzing the generation of free ***,MIPs using sulfamethoxazole as the template was directly prepared on the surface of H-GNs without any film *** importantly,the template could be absorbed on the H-GNs to enhance the number of imprinted sites per unit surface area,which could improve the selectivity of MIPs ***,the composites could exhibit high adsorption capacity(29.4 mg/g),imprinting factor(4.2)and excellent conductivity,which were modified on the surface of electrode for rapid,selective and sensitive detection of sulfamethoxazole in food and serum *** linear range was changed from 5μg/kg to 1 mg/g and the limit of detection was 1.2μg/*** sensor was free from interference caused by analogues of sulfamethoxazole,which provides a novel insight for the preparation of MIPs-based sensor and its application in food safety monitoring and human exposure study.

关键词： MIP/H-GNs composites sulfamethoxazole nano enzyme-mediated polymerization sensor dietary exposure

Determination of Rotenone Residues in Foodstuffs by Solid-Phase Extraction (SPE) and Liquid Chromatography/Tandem Mass Spectrometry (LC-MS/MS)

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Agricultural Sciences in China 2010年第9期9卷 1299-1308页

作者： XU Dun-ming ZHOU Yu LIN Li-yi ZHANG Zhi-gang ZHANG Jin LU Sheng-yu YANG Fang HUANG Peng-ying Xiamen entry-exit inspection and quarantine bureau Xiamen 361026 P.R. China Fujian entry-exit inspection and quarantine bureau Fuzhou 350001 P.R.China

We developed a novel approach to determine rotenone residues in foodstuffs, by integrating solid-phase extraction （SPE） and liquid chromatography/tandem mass spectrometry （LC-MS/MS） technologies, to achieve high sensitivity and selectivity. In our method, the solvent extraction with n-hexane-dichloromethane （50：50, v/v） and cleanup with florisil SPE cartridges using ethyl acetate-ethyl ether （25：75, v/v） as eluents provided adequate recovery of rotenone. The detection of rotenone was then carried out by LC-MS/MS using acetonitrile-water with the 0.1% formic acid （w/v） as the mobile phase. The multiple reaction monitoring （MRM） scheme employed in the approach involved the transitions of the precursor ion to three selected product ions, in which one pair for quantification was m/z 395.3 〉 213.2 and the other two pairs for identification were m/z 395.3 〉 192.2 and 395.3 〉 367.0. The limits of quantification （LOQs） of the method ranged from 0.001 to 0.005 mg kg-1 depending on the matrix. Intra- and inter-day precisions （relative standard deviations, RSDs） for rotenone were less than 7.1 and 14.8%, respectively. Results from repetitive analysis suggested good reproducibility of the method for rotenone residue detection. The recoveries at three concentrations （LOQ, 10LOQ and 100LOQ） ranged from 79.3-118.3% in cabbage, potato, onion, carrot, apple, orange, banana, lichee, tea, and Shiitake mushroom. The proposed procedure was then applied to the analysis of 129 real samples collected from Xiamen, Fujian Province, China. The existence of rotenone was found in two tea products with concentrations of 0.012 and 0.016 mg kg-1, respectively. The method has great potential for routine analysis of monitoring rotenone residue in foodstuffs.

关键词： rotenone LC-MS/MS foodstuff residue SPE

Synthesis, Characterization and Crystal Structure of (+)-N-[(3S)-3-(4- fluorophenyl)heptanoyl]bornane-10,2-sultam

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Chinese Journal of Structural Chemistry 2012年第9期31卷 1247-1250页

作者：韩勰汪淼李菲徐媛原曹秀芳 College of Science Huazhong Agricultural University inspection and quarantine Technology Center Hainan Entry-exit Inspection and Quarantine Bureau

The chiral molecule （＋）-N-[（3S）-3-（4-fluorophenyl）heptanoyl]bornane-10,2-sultam （C23H32FNO3S, Mr = 421.56）, a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the orthorhombic space group P212121 with a = 7.9044（11）, b = 11.6680（16）, c = 24.899（3） , V = 2296.4（5） 3, Z = 4, Dc = 1.219 Mg/m3, λ = 0.71073 , μ（MoKα） = 0.172 mm-1 and F（000） = 904. X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat conformation （Fig. 1）. The planes constructed by （（C6）, （C7）, （C8）, （C9）） and （（C4）, （C5）, （C6）, （C9）） form a dihedral angle of 70.3（3）°. The plane of （C1）-（C2）-（C3） forms dihedral angles to the aforementioned planes of 85.9（4） and 89.5（4）°, respectively. The molecules are linked via C-H···O/F interactions.

关键词： (+)-N- [(3S)-3-(4-fluorophenyl)heptanoyl] bornane-10,2-sultam,synthesis crystal structure

Fast Evaluation of Oxidative DNA Damage by Liquid Chromatography-Electrospray Tandem Mass Spectrometry Coupled With Precision-cut Rat Liver Slices

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Biomedical and Environmental Sciences 2007年第5期20卷 386-391页

作者： JIANG YUE PENG WANG YING-HUI LIU JUN-YU WU JIE CHEN REN-XIU PENG Department of Pharmacology College of Basic Medicine Wuhan University Wuhan 430071 Hubei China inspection ＆ quarantine Technical Center Hubei Entry-exit Inspection and Quarantine Bureau Wuhan 430022 Hubei China

Objective To establish a fast and sensitive method for the detection of 8-hydroxy-2’-deoxyguanosine （8-OHdG） in precision-cut rat liver slices by HPLC-MS/MS and to investigate isoniazid （INH） -induced oxidative DNA damage. Methods Precision-cut liver slices （300 μm） were prepared from male rats, and incubated with INH （0.018 mol/L） for 2 h after 1 h preincubation. DNA in the slices was extracted and digested into free nucleosides at 37℃ . The samples were injected into HPLC-MS/MS after the proteins were removed. The level of oxidative DNA damage was estimated using the ratio of 8-OHdG to deoxyguanosine （dG）. Results The limit of detection of 8-OHdG was 1 ng/mL （S/N=3） and the intra-assay relative standard variation was 3.38% when one transition 284.3/168.4 was used as a quantifier and another two transitions 284.3/140.2, 306.1/190.2 as qualifiers. 8-OHdG and dG were well separated, as indicated by elution at 10.02 and 7.37 min, respectively. INH significantly increased the ratio of 8-OHdG to dG in rat liver slices （P〈0.05）. Conclusion 8-OHdG in precision-cut liver slices could be sensitively determined by HPLC-MS/MS. HPLC-MS/MS coupled with precision-cut tissue slices is a fast and reliable analytical technique to evaluate oxidative DNA damage of target tissues caused by procarcinogens and cytotoxins.

关键词： Isoniazid 8-Hydroxy-2'-deoxyguanosine HPLC-MS/MS Precision-cut liver slices

Determination of Tetracyclines in Honey Using Liquid Chromatography with Ultraviolet Absorbance Detection and Residue Confirmation by Mass Spectrometry

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Chinese Journal of Chemistry 2007年第9期25卷 1294-1299页

作者：刘艳徐锦忠丁涛李公海 Food Laboratory Jiangsu Entry-Exit Inspection and Quarantine Bureau Nanjing Jiangsu 210001 China

A determination method has been optimized and validated for the simultaneous analysis of tetracycline （TC）, oxytetracycline （OTC）, chlortetracycline （CTC） and doxycycline （DC） in honey. Tetracyclines （TCs） were removed from honey samples by chelation with metal ions bound to small Chelating Sepharose Fast Flow columns and eluted with Na2EDTA-Mcllvaine pH 4.0 buffers. Extracts were further cleaned up by Oasis HLB solid-phase extraction （SPE）, while other solid-phase extraction cartridges were compared. Chromatographic separation was achieved using a polar end-capped C 18 column with an isocratic mobile phase consisting of oxalic acid, acetonitrile and methanol. LC with ultraviolet absorbance at 355 nm resulted in the quantitation of all four tetracycline residues from honey samples fortified at 15, 50, and 100 ng/g, with liner ranges for tetracyclines of 0.05 to 2 μg/mL. Mean recoveries for tetracyclines were greater than 50% with R.S.D. values less than 10% （n= 18）. Detection limits of 5, 5, 10, 10 ng/g for oxytetracycline, tetracycline, chlortetracycline and doxycycline, respectively and quantitation limits of 15 ng/g for all the four tetracyclines were determined. Direct confirmation of the four residues in honey （2-50 ng/g） was realized by liquid chromatography-tandem mass spectrometry （LC/MS/MS）. The linear ranges of tetracyclines determined by LC/MS/MS were between 5 to 300 ng/mL, with the linear correlation coefficient r〉 0.995. The limits of detection of 1 to 2 ng/g were obtained for the analysis of the TCs in honey.

关键词： tetracyclines honey metal chelate affinity chromatography LC/MS/MS

In vitro Selection of DNA Aptamers and Fluorescence-Based Recognition for Rapid Detection Listeria monocytogenes

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Journal of Integrative Agriculture 2014年第5期13卷 1121-1129页

作者： LIU Guo-qing LIAN Ying-qi GAO Chao YU Xiao-feng ZHU Ming ZONG Kai CHEN Xue-jiao YAN Yi School of Biotechnology and Food Engineering Hefei University of Technology Anhui entry-exit inspection and quarantine bureau

Aptamers are specific nucleic acid sequences that can bind to a wide range of nucleic acid and non-nucleic acid targets with high affinity and specificity. Nucleic acid aptamers are selected in vitro from single stranded DNA or RNA ligands containing random sequences of up to a few hundred nucleotides. Systematic evolution of ligands by exponential enrichment （SELEX） was used to select and PCR amplify DNA sequences （aptamers） capable of binding to and detecting Listeria monocytogenes, one of the major food-borne pathogens. A simplified affinity separation approach was employed, in which L. monocytogenes in exponential （log） phase of growth was used as the separation target. A fluorescently-labeled aptamer assay scheme was devised for detecting L. monoeytogenes. This report described a novel approach to the detection of L. monocytogenes using DNA aptamers. Aptamers were developed by nine rounds of SELEX. A high affinity aptamer was successfully selected from the initial random DNA pool, and its secondary structure was also investigated. One of aptamers named e01 with the highest affinity was further tested in aptamer-peroxidase and aptamer-fluorescence staining protocols. This study has proved the principle that the whole-cell SELEX could be a promising technique to design aptamer-based molecular probes for dectection of pathogenic microorganisms without tedious isolation and purification of complex markers or targets.

关键词： aptamers systematic evolution of ligands by exponential enrichment (SELEX) Listeria monocytogenes,rapid detection

Prediction of the Shearing Property of Worsted Fabrics Using BP Neural Network

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Journal of Donghua University(English Edition) 2006年第6期23卷 47-49页

作者：徐广标张向华王府梅 College of Textiles Donghua University Panyu entry-exit inspection and quarantine bureau

In this paper, three layers of BP neural network were used to model the shearing properties of worsted fabrics. We train the neural network models with 27 kinds of fabrics, and then use 6 kinds of fabrics to validate ... 详细信息

关键词： worsted fabric shearing properties neural network models predictive accuracy.

The Technology Parameters Optimization of Extracting Natural Cellulose Fibers from Eulaliopsis Binata

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Journal of Donghua University(English Edition) 2010年第4期27卷 516-521页

作者：曲丽君郭肖青由瑞华孙亚宁迟德玲 College of Textile and Clothing Qingdao University Shandong entry-exit inspection and quarantine bureau

The extracting process and parameters optimization of Eulaliopsis binata fibers were *** components of Eulaliopsis binata were tested,the cellulose contents was about 45%,and the lignin content was as high as 18.5%.And the components of Eulaliopsis binata fibers were compared with some bast *** analysis of physical and chemical properties related to acid,alkali,and auxiliary agent about cellulose and pectin,and lignin components in Eulaliopsis binata fibers were *** chemical processing was employed to extract Eulaliopsis binata fibers in which NaOH as cooking agent and Na5P3O10 as auxiliary *** universal rotatable composite experiment design was used to get the highly precise regression equations,in which the NaOH concentration,the auxiliary agent Na5P3O10 concentration and the processing time were the main technological *** residual gum content,fiber fineness,fiber strength,and fiber length of Eulaliopsis binata were the evaluation *** on the relation among parameters of extracting process,degumming effect and quality indexs of Eulaliopsis binata fibers,the optimum parameters of extracting process on Eulaliopsis binata fibers can be *** fibers extracted from Eulaliopsis binata can be developed as one kind of natural cellulose fibers suitable for producing various textile products.

关键词： Eulaliopsis binata fibers extracting parameters optimization

Optimal Design of Mountain Bicycle Based on Biomechanics

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Transactions of Tianjin University 2010年第1期16卷 45-49页

作者：卜研黄田项忠霞吴小凡陈春 School of Mechanical Engineering Tianjin University Tianjin entry-exit inspection and quarantine bureau

To achieve better cycling performance and vibration comfort of mountain bicycle, the optimization of frame structural parameters and rear suspension scale parameters is investigated based on ***, the quadratic sum of rider lower limb muscles stresses is presented as the evaluation criterion of muscle *** taking the criterion as the objective function, the relative positions of three pivot points of frame are optimized to ensure that the frame structural parameters match the stature o...

关键词： mountain bicycle biomechanics muscle fatigue vibration comfort optimum design