基于中性解吸-电喷雾萃取电离质谱直接检测蜂蜜中的四环素

基于中性解吸-电喷雾萃取电离质谱(ND-EESI-MS)建立了无需样品预处理即可直接检测蜂蜜中四环素的方法. 测定结果表明, 加标蜂蜜四环素样品在20~1000 ng/mL浓度范围内线性关系良好(R²>0.997), 检出限为1.08 ng/mL; 加标浓度为50, 500和1000 ng/mL蜂蜜样品的回收率分别为94.26%, 98.38%和103.00%, 精密度(RSD)分别为3.28%, 1.39%和1.12%. 应用此方法对8种市售蜂蜜进行检测, 发现2种蜂蜜中含有痕量的四环素, 其余蜂蜜均未检出, 而应用高效液相色法在这8种市售蜂蜜中均未检出四环素. 本方法无需经过复杂的样品预处理, 灵敏度高、 精密度好、 分析速度快且特异性强, 能够承受蜂蜜中复杂基体的影响, 是一种快速检测蜂蜜中四环素的方法.     

Ultraviolet Light Assisted Hierarchical Porous Fe2O3 Catalyzing Heterogeneous Fenton Degradation of Tetracycline Under Neutral Condition with a Low Requirement of H2O2

The hierarchical porous Fe2O3 particles as a novel ultraviolet light assisted heterogeneous Fenton catalysts were synthesized by bio-template synthesis method using iron nitrate as precursor at high temperature of around 550℃.The hierarchical porous structured Fe2O3 was endowed with a large surface area and abundant pore volume,leading to the exposure of more active sites and rapid mass transfer.The synergistic effect of UV irradiation and hie-rarchical porous Fe2O3 improved the photo-degradation efficiency of Tetracycline(TC).The degradation efficiency of Fe203 catalyzing UV-Fenton system reached 97.4%after 60 min reaction,which was more substantial than Fe2O3 catalyzing Fenton system(7.6%)and UV/H2O2 system(59.2%).Moreover,the hierarchical porous Fe2O3 catalyzing UV-Fenton system exhibited an extremely wide pH range(from 3.0 to 9.0,from mildly acidic to slightly alkaline)for efficient degradation of TC.Simultaneously,the extraordinary higher degradation efficiency was based on 10 mmol/L H2O2 concentration,which was low requirement for H2O2,Further,the hierarchical porous Fe2O3 can be used for five consecutive cycles with over 95%of the original degradation efficiency.Ultraviolet light assisted heterogeneous Fenton reaction in the hierarchical porous Fe2O3 improved the·OH and O2·^-production and Fe(III)/Fe(II)redox cycle,which consequently achieved an excellent degradation rate.     

四环素在海洋沉积物上的吸附

研究了四环素在不同pH、盐度、温度下在海洋沉积物上的吸附特征. 结果表明, 在实验浓度范围内吸附行为都可以用线性等温式进行描述. 通过一种包含四环素3种形态与沉积物界面相互作用的模型对不同pH下的吸附常数进行拟合, 发现四环素正价态的吸附常数K_d⁺远大于中性态的K_d⁰与负价态的K_d^-. 随着盐度的减小四环素在海洋沉积物上的吸附增强, 而温度的升高则不利于吸附的进行. 热力学计算结果得出, ΔG^0-=-9.746~-9.713 kJ/mol; ΔH^0-=-10.056 kJ/mol; ΔS^0-<0, 表明该吸附过程是一个自发的、放热的熵减过程.     

Label-free fluorescent strategy for sensitive detection of tetracycline based on triple-helix molecular switch and G-quadruplex

In this assay, a label-free fluorescent sensing platform based on triple-helix molecular switch (THMS) and G-quadruplex was developed for the detection of tetracycline. We demonstrated this approach by using THMS, which consists of a central section with a shortened 8-mer aptamer sequence with high affinity to tetracycline and flanked by two arm segments. G-rich oligonucleotide can specifically bind to thioflavin T (ThT) as a signal transduction probe (STP). In the absence of tetracycline, THMS remains stable, the fluorescence of background is low. By the addition of target tetracycline, the aptamer-target binding results in the formation of a structured aptamer-target complex, which disassembles the THMS and releases the STP. The free STP self-assembles into G-quadruplex and specifically binds to ThT which generates a obvious fluorescence enhancement. Using the triple-helix molecular switch, the developed aptamer-based fluorescent sensing platform showed a linear relationship with the concentration of tetracycline ranging from 0.2 to 20.0 nmol/L. The detection limit of tetracycline was determined to be 970.0 pmol/L. The assay avoids complicated modifications or chemical labeling, making it simple and cost-effective. So, it is expected that this aptamer-based fluorescent assay could be extensively applied in the field of food safety inspection.     

微流动注射芯片化学发光法检测鱼虾中的四环素

四环素(tetracycline,TC)是广谱类抗生素,由于价格低廉,防病和抗病能力强,被许多人用于食用动物和海洋生物的养殖中,由此造成动物组织中四环素的残留,人们长期食用这种动物及制品,会对人类健康构成严重的威胁。分析四环素类抗生素残留量的方法包括微生物法、紫外法、薄层色谱法     

高效液相色谱法测定化妆品中九种禁用四环素类抗生素的方法研究

建立了用反相高效液相色谱法同时测定化妆品中9种禁用四环素类抗生素. 采用甲醇超声提取, Kromasil C18柱(250 mm×4.6 mm i.d., 5 μm)分离测定. 9种被测物在12 min内均得到良好的分离. 在1～100 μg/mL范围内均与其各自对应的峰面积呈良好线性关系(r≥0.9991), 回收率在85.5%～105.7%之间, 精密度RSD＜3.2%, 该方法的检出限(S/N=3)为0.05～0.5 μg/mL. 该法可用于祛痘类化妆品中9种禁用四环素类抗生素的检测.     

Synthesis of Tetracycline Analogues and Test of Their Affinity on Synthetic Hydroxyapatite

To develop bone target drugs is an attractive field for increasing the potency and selectivity of these drugs in the treatment of osteoporosis and Pagets disease etc. As known, after systematic administration tetracycline can be distributed in bone and bind to hydroxyapatite with high affinity1. Thus we tried to use tetracycline as a bone targeted carrier. However, tetracycline is less stable, and its complex structure bring much difficulty in the coupling reaction and purification of the p…     

Voltammetric studies on composition and stabilities of complexes of tetracycline and oxytetracycline with some metal ions in aqueous medium

Summary The composition and stability of complexes of tetracycline and oxytetracycline with Cu(II), Cd(II), Pb(II) and UO₂(II) have been studied polarographically (direct current and differential pulse polarographic techniques) at 25±0.1°C. Differential pulse polarographic studies have been particularly helpful in deciding the nature of metal-drug interactions at low concentrations. The reduction of Cu(II)-tetracycline has been found to be irreversible and diffusion controlled with the presence of an adsorption component. In the system uranyl(II)-tetracycline the complex formed has a stoichiometry of 1:1 and logK _ox=4.04 which is very close to that obtained by potentiometric measurements. The peak half widthW _1/2 of the Pb(II)-OTC system is 60 – 70mV indicating that the process is reversible and two electrons are consumed. The log is 10.30 in 0.1 mol dm^–3 NaClO₄. In the Cu(II)-OTC system two complexes were formed with log ₁=8.50 and log ₂=14.10. Cyclic voltammograms were recorded using a hanging dropping mercury electrode for the systems Cu(II), Cd(II), Pb(II) and UO₂(II)-OTC to examine the irregularities in both peak potentials and peak currents during the polarographic investigations.

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Voltammetrische Untersuchungen zur Zusammensetzung und Stabilität von Komplexen von Tetracyclin und Oxytetracyclin mit einigen Metallionen in wäßrigem Medium

Zusammenfassung Es wurden Zusammensetzung und Stabilität von Tetracyclin- und Oxytetracyclin-Komplexen mit Cu(II), Cd(II), Pb(II) und UO₂(II) polarographisch mittels Direktstrom- und differentieller Pulspolarographie-Technik bei 25±0.1°C bestimmt. Zur Aufklärung der Metall-Substrat-Wechselwirkungen bei geringen Konzentrationen waren insbesonders differentielle Pulspolarographie-Untersuchungen erfolgreich. Es wurde festgestellt, daß die Reduktion von Cu(II)-Tetracyclin irreversibel und diffusionskontrolliert verläuft. Im System Uranyl(II)-Tetracyclin hat der Komplex eine Stöchiometrie von 1:1 und ein logK _oxvon 4.04; dieser Wert ist dem aus potentiometrischen Messungen erhaltenen sehr ähnlich. Die Peak-Halbwertsbreite des Pb(II)-OTC-Systems ist 60 – 70 mV und zeigt damit einen reversiblen Prozess bei Verbrauch von zwei Elektronen an. In 0.1 mol dm^–3 NaClO₄ ist log 10.30. Im Cu(II)-OTC-System werden zwei Komplexe mit log ₁=8.50 und log ₂=14.10 gebildet. Die cyclischen Voltammogramme wurden unter Verwendung einer hängenden tropfenden Quecksilberelektrode für die Systeme Cu(II), Cd(II), Pb(II) und UO₂(II)-OTC aufgenommen, um die Unregelmäßigkeiten der Peak-Potentiale und der Peak-Ströme während der polarographischen Untersuchung zu überprüfen.

     

同步荧光法同时测定四环素和脱水四环素

本文提出了同步荧光法同时测定四环素（ＴＣ）和脱水四环素（ＡＴＣ）新方法。ＴＣ和ＡＴＣ与铝离子形成络合物后分别在３８７／４６２ｎｍ和４８０／５３８ｎｍ处发射增强的荧光；加入十二烷基硫酸钠（ＳＬＳ）后，ＴＣ和ＡＴＣ络合物的荧光强度分别增强４．５倍和８倍。其同步荧光峰在△λ＝６０ｎｍ时完全分离，在ＴＣ和ＡＴＣ浓度比为２０：１～１：２０范围内可同时测定ＴＣ和ＡＴＣ。本法测定尿液中ＴＣ和ＡＴＣ的回收率为９４     

Simple Liquid Chromatographic Determination of Minocycline in Brain and Plasma

A new high-performance liquid chromatography assay was developed for the determination of minocycline in plasma and brain. A solid–liquid extraction procedure was coupled with a reversed-phase HPLC system. The system requires a mobile phase consisting of acetonitrile:water:perchloric acid (26:74:0.25, v/v/v) adjusted to pH 2.5 with 5 M sodium hydroxide for elution through a RP8 column (250 × 3.0 mm, i.d.) with UV detection set at 350 nm. The method proved to be accurate, precise (RSD < 20%) and linear between 0.15–20 μg mL⁻¹ in plasma and 1–20 μg mg⁻¹ in brain. The method was successfully applied to a blood-brain barrier minocycline transport study.