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1.
应用超高效液相色谱串联质谱建立鸡蛋中加雷沙星、曲伐沙星、莫西沙星、奥比沙星、吉米沙星、加替沙星、培氟沙星和环丙沙星等22种喹诺酮类药物残留检测方法。样品经过2%甲酸乙腈提取、正己烷分步去脂,Oasis HLB柱净化后,经Acquity UPLC BEH Shield RP18(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,双通道MRM信号采集模式,22种喹诺酮类药物能在11 min完好分离,方法的最低定量限均低于1.0μg/kg,在2.0~100.0μg/L浓度范围内,22种喹诺酮类药物线性良好,相关系数均在0.99以上;通过2、10、20 g/kg三个浓度的加标回收实验表明,回收率为60.1%~96.2%,RSD%值为1.44%~11.1%。该方法相比现有国标检测药物种类多,新型药物多,对更全面筛查和确证鸡蛋中喹诺酮类药物残留,防范非法添加造成安全隐患具有一定的参考价值。  相似文献   
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A multiresidue method has been developed for the confirmation and quantification of 19 quinolones (enrofloxacin, ciprofloxacin, norfloxacin, ofloxacin, flumequine, oxolinic acid, difloxacin, sarafloxacin, sparfloxacin, danofloxacin, fleroxacin, marbofloxacin, enoxacin, orbifloxacin, pefloxacin, nalidixic acid, pipemidic acid, lomefloxacin and cinoacin) in pig and fish by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile, analytes separated by LC on a C18 column using 0.1% formic acid–methanol with a linear gradient elution programme, and detected by MS/MS. The linear range was 0.3–50 µg kg–1 with correlation coefficients (r) more than 0.9956. The limits of detection were 0.1 µg kg–1. Mean recoveries for each analyte in pig muscle and fish ranged from 75.3% to 96.3% and from 79.7% to 94.2% with relative standard deviations below 10%. The method is fast, safe, sensitive and precise, and can be used simultaneously to analyse residual quinolones.  相似文献   
4.
For rapid and simultaneous detection of (fluoro)quinolones, a broadly specific monoclonal antibody (mAb) that recognizes 32 (fluoro)quinolone antibiotics was prepared using a mixture of a norfloxacin derivative and a sarfloxacin derivative as the hapten. An immunochromatographic strip based on gold nanoparticles (AuNPs) was then assembled with goat anti-mouse antibody and antigen (sarfloxacin coupled to ovalbumin), used to form the C line and T line, respectively. This antigen competes with the (fluoro)quinolones in a sample incubated with mAbs labeled with AuNPs. The strip can detect 32 (fluoro)quinolones including oxolinic acid, nalidixic acid, miloxacin, pipemidic acid, piromidic acid, rosoxacin, cinoxacin, norfloxacin, pefloxacin, lomfloxacin, enofloxacin, fleroxacin, ciprofloxacin, enrofloxacin, dafloxacin, orbifloxacin, sparfloxacin, gemifloxacin, besifloxacin, balofloxacin, gatifloxacin, moxifloxacin, nadifloxacin, ofloxacin, marbofloxacin, flumequine, pazufloxacin, prulifloxacin, sarafloxacin, difloxacin, trovafloxacin, and tosufloxacin in milk within 10 min with the naked eye. The cut-off values of the strip range from 1 to 100 ng/mL and the limits of detection are 0.1–10 ng/mL. The strip does not cross-react with antibiotics including tetracycline, sulfamethazine, ampicillin, erythromycin, aflatoxin B1, or gentamicin. In short, this immunochromatographic strip is a very useful tool for the primary screening of (fluoro)quinolones in milk.
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Campylobacter spp. genera is one of the most common causes of microbial enteritis worldwide. The objective of this work was to investigate the antimicrobial resistance (AMR) patterns, virulence genes, and genetic variation of thermophilic Campylobacter species collected from chicken meat samples in Iran. A total of 255 meat specimens were taken and transferred to the laboratory. Culture methods were utilized to identify the Campylobacter genus, and PCR and sequencing were performed to confirm the organisms. Antimicrobial susceptibility evaluation was performed using broth microdilution for six antimicrobials [ciprofloxacin (CIP), nalidixic acid (NAL), sitafloxacin (SIT), erythromycin (ERY), tetracycline (TET), and gentamicin (GEN)]. By using PCR, AMR and virulence genes were detected. The detection rate of Campylobacter spp. was 64 (25.09%) out of 255 meat samples, with C. jejuni and C. coli accounting for 41 (64.06%) and 14 (21.87%), respectively. Other Campylobacter isolates accounted for 14.06% of the total (nine samples). The antibiotic susceptibility of all Campylobacter isolates was tested using six antibiotics, and all (100%) were resistant to CIP and NAL. However, TET resistance was observed in 93.9% and 83.3% of C. jejuni and C. coli isolates, respectively. Four (8.2%) C. jejuni isolates were multidrug-resistant (MDR), while none of the C. coli isolates were MDR. Two of the four MDR isolates were resistant to CIP, NAL, TET, and ERY, whereas the other two isolates were resistant to CIP, NAL, TET, and GEN. The values of the Minimum Inhibitory Concentration (MIC) were as follows: CIP, 64–256 μg/ml; NAL, 128–512 μg/ml; TET, 2–1024 μg/ml; SIT, 0.25–1 μg/ml; ERY, 1–32 μg/ml; and GEN, 1–256 μg/ml. recR, dnaJ, cdtC, cdtB, cdtA, flaA, ciaB, cadF, and pidA were discovered in more than 50% of C. jejuni isolates, although wlaN, virbll, cgtB, and ceuE were found in <50%. flaA, cadF, pidA, and ciaB were discovered in more than 50% of the C. coli samples, whereas recR, cdtC, cdtB, cdtA, and cgtB were found in less than half. For C. coli, the percentages for wlaN, dnaJ, virbll, and ceuE were all zero. The results of this study show Campylobacter isolates obtained from poultry have higher resistance to quinolones and TET, pathogenicity potential, and varied genotypes.  相似文献   
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4‐Aryl‐2(1H)‐quinolones were efficiently synthesized via copper‐catalyzed hydroarylation of (o‐aminophenyl)propiolates with arylboronic acid neopentyl glycol esters. The substrate propiolates were prepared from the corresponding silylalkynes with carbon dioxide by Kondo’s carboxylation method using N,N‐dimethylformamide as a solvent. Hydroarylation was performed in the presence of 3 mol% copper(II) acetate in methanol at 28 °C for 12 h and subsequent deprotection using trifluoromethanesulfonic acid (3.0 equiv.) at 65 °C for 2 h in the same pot to afford the desired 4‐aryl‐2(1H)‐quinolones in 39–89% yields.

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7.
    
A series of 1,2‐ and 1,4‐dihydroquinolines has been successfully prepared. The Pd‐catalyzed intramolecular N‐arylation of Z‐enamines, formally prepared by the Horner–Wadsworth–Emmons olefination, proceeded efficiently to furnish the cyclized products. Depending on the cyclization conditions, substituted 1,4‐dihydroquinolines and further isomerized 1,2‐dihydroquinolines were independently obtained in high yields with an excellent control of isomerization of the double bond.

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8.
本文旨在建立一种可检测牛奶中喹诺酮类药物(Quinolones,QNS)残留的均相光激化学发光免疫分析方法(Amplifiedluminescent proximity homogeneous assay linkedimmune sorbent assay,AlphaLISA)。采用EDC/NHS活泼酯法在诺氟沙星分子连接6-氨基己酸作为间隔臂,制备生物素修饰诺氟沙星半抗原(Biotin-6AS-NOR),并在受体微球上偶联QNS单克隆抗体,Biotin-6AS-NOR可与牛奶样品中的QNS竞争结合喹诺酮抗体;通过优化受体微球的QNS抗体偶联量,Biotin-6AS-NOR及供/受体微球的用量等参数,以及牛奶样品的稀释方案,建立了牛奶中QNS残留的AlphaLISA检测方法。采用1:5牛奶样品稀释方案,所建立牛奶中QNS残留的AlphaLISA检测方法的检出限和定量限分别为0.19 ng/mL和0.46 ng/mL,回收率在85.97%~110.11%之间,日内和日间变异系数均小于10%,与诺氟沙星、恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、达氟沙星和洛美沙星的交叉反应率均高于70%。本研究所建立AlphaLISA检测方法具有灵敏度和准确度高、重复性好等优点,且在整个检测过程中不需要繁琐洗涤操作,具有较高的应用和推广价值。  相似文献   
9.
目的 建立一种检测8种喹诺酮类抗生素的液相色谱-串联质谱法并评价其在水体环境中的应用。方法 采用C18色谱柱(10 mm×2.1 mm,1.7 μm)为分离柱,以甲醇~0.1%甲酸水溶液为流动相,设定柱温为35 ℃、流速为0.35 mL/min;质谱条件采用电喷雾离子源 (Electron Spray Ionization, ESI) 正离子模式(ESI+)及多反应监测(multiple reaction monitoring, MRM)模式采集。结果 在0.1~100.0 μg/L浓度范围内,马波沙星、氧氟沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星6种抗生素的质量浓度与峰面积线性关系良好(r2>0.99), 检出限为0.1 μg/L; 在5.0~500.0 μg/L浓度范围内,培氟沙星、诺氟沙星的质量浓度与峰面积线性关系良好(r2>0.99),检出限为5.0 μg/L。8种喹诺酮在环境水样品中的平均回收率为98.30%~111.77%,相对标准偏差为0.71%~12.80%。结论 该方法简单、灵敏、准确,可以满足水体环境中喹诺酮类抗生素检测。  相似文献   
10.
Lv K  Sun Y  Sun L  Wei Z  Guo H  Wu J  Liu M 《ChemMedChem》2012,7(7):1230-1236
A series of novel (R)/(S)-7-(3-alkoxyimino-2-aminomethyl-1-azetidinyl)fluoroquinolone derivatives were synthesized and evaluated for their in vitro antibacterial activity against representative strains. Our results reveal that 12 of the target compounds generally show better activity (MIC: <0.008-0.5 μg mL(-1)) against the tested Gram-positive strains including MRSA and MRSE than levofloxacin (LVFX, MIC: 0.125-8 μg mL(-1)). Their activity is similar to that of gemifloxacin (GMFX, MIC: <0.008-4 μg mL(-1)). However, they are generally less active than the two reference drugs against Gram-negative strains. Moreover, against clinical strains of S. aureus including MRSA and S. epidermidis including MRSE, the MIC(50) values (0.06-16 μg mL(-1)) and MIC(90) values (0.5-32 μg mL(-1)) of compounds 16 w, y, and z are 2-8- and 2-16-fold less than LVFX, respectively, and 16 w (MIC(90) range: 0.5-4 μg mL(-1)) was also found to be more active than GMFX (MIC(90) range: 1-8 μg mL(-1)).  相似文献   
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