Indirect Flow Injection Chemiluminescence Method for the Determination of Tetracycfines Using Cu（]I） as a Probe Ion

This paper reported an indirect flow injection chemiluminescence （FI-CL） method for the determination of the drugs tetracycline （TC）, chlortetracycline （CTC） and oxytetracycline（OTC） using Cu（ Ⅱ ） as a probe ion. The CL reaction was induced on-line and after injection of the sample the negative peaks appeared as a result of complexation. The method was applied to the determination of TCs in pharmaceuticals and human urine with recoveries in the range95-105%.     

STUDIES ON THE ADSORPTION OF ANTIBIOTICS OF THE TETRACYCLINE GROUP ONTO SULFOCATIONITES

The adsorption processes of antibiotics of the tetracyline group (ATG) by several home-made sulfocationites are studied in this paper.The results show that the adsorption may be of nonequivalent normality under certain pH condition.The adsorption mechanism is discussed with infrared spectrometry.It can be concluded that ATG can interact with sulfocationites by ion exchange mechanism or ion-transfer mechanism or both of them.     

四环素类药物残留检测技术取得突破

前不久，由深圳检验检疫局承担的国家“十五”食品安全重大专项“兽药残留检测技术研究”子课题“四环素类兽药多残留检测技术研究”项目通过了国家质检总局有关专家的鉴定。     

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

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.     

镉-铽-铕-强力霉素-曲通X-100协同荧光增敏体系研究

研究了在表面活性剂TritonX 10 0存在下 ,稀土离子和部分主、副族元素的离子对Eu 强力霉素(DC)体系的协同荧光增敏效应 ,建立了Cd Tb Eu DC TritonX 10 0协同荧光增敏体系 ,并提出了一种高灵敏度测定稀土元素铕的荧光光度新方法。方法的检出限为 5 .0× 10 -11mol/L ;线性范围为 4 .0× 10 -10 ～ 4 .0× 10 -8mol/L。     

固相萃取–超高效液相色谱三重四级杆质谱联用法测定水中四环素、土霉素及罗红霉素

建立了固相萃取–超高效液相色谱三重四级杆质谱联用法同时测定水中的罗红霉素、四环素和土霉素残留。水样经过固相萃取纯化、富集,液质联用分析,采用甲酸溶液和乙腈作为流动相,在5 min内完成对3种目标化合物的分析,3种目标化合物的方法检出限介于0.08~0.35 ng/L之间,测定结果的相对标准偏差为1.4%~5.6%,空白样品和实际样品的加标回收率分别为82.5%~114%,71.5%~126%。     

四级杆飞行时间串联质谱高通量筛查鱼肉中的药物残留

建立了以QuEChERS样品预处理方法、四级杆飞行时间串联质谱(Q-TOF MS)为检测手段,针对鱼肉中的四环素类、磺胺类、喹诺酮类、三苯甲烷类、雄激素、孕激素和糖皮质激素7类59种残留药物的快速筛查技术。通过正交实验得到优化条件为:Na2EDTA-Mcllvaine为缓冲溶液,乙腈为提取剂,净化剂无水MgSO4、十八烷基键合硅胶(C18)和N-丙基乙二胺(PSA)的用量分别为每毫升提取液加入25,12.5和6.25 mg。对Q-TOF质谱筛查出的阳性样品,再用LC-MS/MS对样品进行确证。本方法对59种药物的检出下限为0.5~5.3μg/kg。本方法快速、简单、可靠,可筛查的渔药种类覆盖面广,灵敏度满足水产品药物残留检测的要求,适用于鱼类水产品中残留药物的快速测定。     

g-C3N4/CeO2异质结材料的制备及其光催化性能的研究

以三聚氰胺、硝酸铈为原料,通过高温煅烧法制备了不同CeO₂含量的片层状g-C₃N₄/CeO₂,通过XRD、FT-IR、XPS等对系列g-C₃N₄-CeO₂材料进行了表征,考察了材料在可见光(λ≥420nm)条件下降解盐酸四环素(TC)的光催化活性。与单纯的g-C₃N₄相比,g-C₃N₄/CeO₂-30%具有更优异的光催化性能,这是由于g-C₃N₄-CeO₂间的异质结作用促进了光生电子和空穴分离。自由基捕获实验证实·O^-₂在催化反应过程中起到主要作用,并提出了相应的光催化机理。     

四环素类抗生素药物的发现、发展与合成:源于天然产物,用于人类健康

四环素类抗生素是一类广谱抗生素,广泛应用于治疗由革兰阳性和阴性细菌、支原体、衣原体和立克次氏体感染所引起的疾病.四环素类抗生素药物由ABCD四个六元并环骨架结构所构成.目前,人们主要通过发酵途径获得四环素类天然抗生素,再通过化学半合成的方式对其进行结构改造,其中A环取代方式固定,人们主要对D环作结构改造以获得临床药效更加优异的非天然新型四环素类抗生素药物.自1962年四环素Sancycline全合成工作以来,合成工作者们完成了多个四环素类抗生素药物的全合成,如近年通过发展新颖合成策略完成了四环素类抗生素药物Doxycycline的全合成;其后,人们通过全合成高效地完成了其他四环素类抗生素药物的合成和结构改造,加速了新型四环素类抗生素药物的研发与上市.本综述归纳总结了四环素类药物的发现和发展史,并介绍了其生物合成机制和针对病原菌的药物作用模式,详细介绍并比较了各种四环素类药物的半合成和全合成方式,将为研究者了解四环素抗生素及其结构类似药物的发现、发展和合成空间等起到有益作用.     

铕-四环素-TOPO-十二烷基磺酸钠荧光体系及四环素测定的研究

广谱抗菌素四环素是一种亲癌化合物,近年来已成为诊断、治疗肿瘤的一种重要的荧光探针,并用于临床检查和治疗中。已报道的检测四环素的极谱、比色、色谱、紫外分光光度、荧光和微生物等法大多复杂且费时。而四环素能与Eu~(3+)形成稳定螯合物,且四环素-Eu~(3+)-TOPO-十二烷基磺酸钠多元络合物体系能发射很强的Eu~(3+)的特征荧光,所以我们提出了用上述多元络合物荧光体系来检测四环素的新的荧光方法,并将该法用于人体血清和尿中四环素的测定。结果表明,该法的检出限为1.2×10~(-8)mol/L,比Eu~(3+)-四环素二元荧光体系的灵敏度约提高两个数量级,且具有简便、快速等特点。