Quantification of clenbuterol in equine plasma,urine and tissue by liquid chromatography coupled on-line with quadrupole time-of-flight mass spectrometry

Clenbuterol (CBL) is a potent beta(2)-adrenoceptor agonist used for the management of respiratory disorders in the horse. The detection and quantification of CBL can pose a problem due to its potency, the relatively low dose administered to the horse, its slow clearance and low plasma concentrations. Thus, a sensitive method for the quantification and confirmation of CBL in racehorses is required to study its distribution and elimination. A sensitive and fast method was developed for quantification and confirmation of the presence of CBL in equine plasma, urine and tissue samples. The method involved liquid-liquid extraction (LLE), separation by liquid chromatography (LC) on a short cyano column, and pseudo multiple reaction monitoring (pseudo-MRM) by electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS). At very low concentrations (picograms of CBL/mL), LLE produced better extraction efficiency and calibration curves than solid-phase extraction (SPE). The operating parameters for electrospray QTOF and yield of the product ion in MRM were optimized to enhance sensitivity for the detection and quantification of CBL. The quantification range of the method was 0.013-10 ng of CBL/mL plasma, 0.05-20 ng/0.1 mL of urine, and 0.025-10 ng/g tissue. The detection limit of the method was 13 pg/mL of plasma, 50 pg/0.1 mL of urine, and 25 pg/g of tissue. The method was successfully applied to the analysis of CBL in plasma, urine and various tissue samples, and in pharmacokinetic (PK) studies of CBL in the horse. CBL was quantified for 96 h in plasma and 288 h in urine post-administration of CLB (1.6 micro g/kg, 2 x daily x 7 days). This method is useful for the detection and quantification of very low concentrations of CBL in urine, plasma and tissue samples.     

Neutron activation analysis of gold and iridium in steel

A method of determination of trace gold and iridium in steel is presented. The samples were preconcentrated with an anion exchanger. The chemical recoveries were determined by an isotope tracer technique using¹⁹⁸Au and¹⁹²Ir.     

POLYMER NETWORK-POLY(ETHYLENE GLYCOL)COMPLEXES WITH SHAPE MEMORY EFFECT

The complexes of poly(methacrylic acid-co-methyl methacrylate) network with poly(ethylene glycol) stabilized byhydrogen bonds were prepared. By introducing the poly(ethylene glycol), a large difference in storage modulus below andabove the glass transition temperature occurred and the complexes exhibited shape memory behaviors. The morphology ofcomplexes was studied by using DSC, WAXD, and DMA. The results indicate that the fixed phase of this kind of novelshape memory materials is the network, and the reversible phase is the amorphous state of PEG:PMAA complex phase. Theshape recoverability almost reaches 100%. This type of complexes can be regarded as a novel shape memory network.     

火焰原子吸收光谱法测定茶叶中的锰

介绍悬浮液进样-次灵敏线火焰原子吸收光谱法测定茶叶中的锰的方法。以琼脂为悬浮剂，将茶叶样品均匀、稳定地悬浮于琼脂溶胶中，直接喷入空气-乙炔火焰中，利用锰280.1nm次灵敏线，以工作曲线或标准加入法测定锰的含量，方法简便、快速，用于测定茶叶和桃叶样品中的锰，结果准确。     

离子交换树脂负载Ni—B无定形合金催化剂的制备与性能

制备了一种新型离子交换树脂负载的Ｎｉ－Ｂ无定形合金催化剂．用３种树脂作为催化剂载体，即弱酸型阳离子树脂Ｄ１５２，强酸型阳离子树脂Ｄ７２及强碱型阴离子树脂Ｄ２６１．用ＸＰＳ、ＴＥＭ和ＩＣＰ等技术对催化剂进行了表征．结果表明，催化剂上镍与带有功能基的载体树脂之间有着很强的相互作用，但其强度与所带的功能基有关．３种催化剂Ｎｉ２ｐ３／２的ＸＰＳ谱图上，ＮｉＢ／Ｄ１５２催化剂的氧化态峰最小，而ＮｉＢ／Ｄ２６１的氧化态峰最大．异丙醇脱氢反应活性实验证实了这一结果．     

生物检材中乌头类生物碱的检验

 用薄层 (TLC)、高效液相 光电二极管阵列检测器 (HPLC/DAD)、动物实验等方法对生物检材中乌头生物碱进行检验 ,并对这些方法进行比较。结果发现 ,TLC法为此类药物检验筛选的首选方法 ,最小检出量为 0 3μg。在进行HPLC检测时 ,以乌头生物碱的特征紫外吸收光谱和动物实验结果为重要的定性手段 ,其特征吸收波长为 (2 2 8± 2 )nm和 (2 75± 2 )nm。乌头生物碱在 2mg/L～ 5 0mg/L时其峰面积与质量浓度有很好的线性 ,相关系数为 0 9996。经实际案件证明 ,方法准确、灵敏 ,可用于生物检材中乌头类生物碱的检验。     

微型集成化色谱仪

用微制造技术和色谱原理结合，以全新的概念和设计思维研制色谱仪一微型集成化色谱仪。这种仪器的整个色谱部分在基片上制成。集微型进样器，细内径毛细管柱和微型固体检测器于一体，功耗不过几瓦，重不过几百克，而分析速度比现有仪器提高近一个数量级，检测灵敏度可达１０＾－６Ｖ／Ｖ。这种仪器的制作过程类似半导体器件，能大批量，性能高度重复可靠、而成本极为低廉地制造出来，彻底改变传统色谱仪器的生产方式。本文给出这种仪     

CdS nanocrystallites sensitized ZnO nanorods with plasmon enhanced photoelectrochemical performance

A sandwiched structure of CdS/Ag/ZnO nanorod photoanode exhibits greatly enhanced photoelectrochemical activity for solar hydrogen generation, due to synergistic effect of CdS nanocrystallites and plasmonic Ag nanoparticles for the enhanced optical absorption and the promoted charge carrier separation.     

毛细管气相色谱法同时测定水产品中的多氯联苯和有机氯农药残留量

建立了毛细管气相色谱法同时测定水产品中多氯联苯和有机氯农药的方法，用高氯酸与冰乙酸的混合溶液消化样品，以石油醚提取，浓硫酸净化后，用毛细管气相色谱法测定，方法的回收法为88％－110％，相对标准偏差为8％－19％（n=6)，检出限为0．08－0．60ug/kg，方法简便，快速，结果准确。