固相萃取-高效液相色谱/串联质谱法测定食醋中的3种甜味剂

建立了食醋中3种甜味剂的固相萃取-高效液相色谱/串联质谱分析方法。样品经酸性水稀释,弱阴离子固相萃取柱净化,Pursuit C18色谱柱分离,10 mmol/L醋酸铵(含0.1%氨水)和乙腈为流动相梯度洗脱,电喷雾负离子模式下多反应监测(MRM)模式检测。糖精钠、安赛蜜、甜蜜素的定量限分别为10、5、5 μg/kg,回收率为72.1%～96.8%,相对标准偏差小于15%。该方法准确、灵敏度高,可用于食醋中甜味剂的定性定量检验。     

黄连生物碱的反相高效液相-电喷雾离子阱串联质谱的研究

采用反相高效液相-电喷雾离子阱串联质谱法对由乙醇提取的黄连生物碱进行了研究.优化出了反相高效液相色谱分离黄连生物碱的条件:流动相为V(乙腈):V(H2O)(三乙胺2 mmol/L)=30:70;柱温为30℃;流速为0.5 mL/min,并结合电喷雾串联质谱检测出了黄连生物碱中的小檗碱、药根碱、巴马汀、黄连碱以及微量的表...     

Liquid Phase Hydrogenolysis of Biomass‐derived Lactate to 1,2‐Propanediol over Silica Supported Cobalt Nanocatalyst

Liquid phase hydrogenolysis of ethyl lactate to 1,2‐propanediol was performed over silica supporting cobalt catalysts prepared by two different methods: precipitation‐gel (PG) technique and deposition‐precipitation (DP) procedure. The cobalt species (Co₃O₄/cobalt phyllosilicate) present in the corresponding calcined PG and DP catalysts were different as a consequence of the preparation methods, and Co OH Co olation and Si O Co oxolation molecular mechanisms were employed to elucidate the chemical phenomena during the different preparation procedures. In addition, the texture (BET), reduction behavior (TPR and in‐situ XRD), surface dispersion and state of cobalt species (XPS), and catalytic performance differ greatly between the samples. Because of small particle size, high dispersion of cobalt species and facile reducibility, the Co/SiO₂ catalyst prepared by precipitation‐gel method presented a much higher activity than the catalyst prepared by deposition‐precipitation method. Metallic cobalt is assumed to be the catalytically active site for the hydrogenolysis reaction according to the catalytic results of both cobalt samples reduced at different temperatures and the structure changes after reaction.     

Effect of Temperature on Self‐Interaction of Human‐Like Collagen

Effects of temperature on self‐interaction of human‐like collagen (HLC) were investigated by hydrophobic interaction chromatography, calorimetric measurement, and sodium dodecyl sulphate‐polyacrylamide gel electrophoresis (SDS‐PAGE) analysis. Results show that three types of interaction roles may exist between HLC molecules at 3–50°C, which were divided into three narrower temperature ranges. In temperature range from 3–22°C, hydrogen bonding plays a key role in the formation of a gelatinous aggregate. In the range of 22–38°C, hydrophobic bonds accompanied by hydrogen bonds are involved in the formation compact aggregates. When temperature is above 38°C the hydrophobic effect formed in the HLC monomer results in the loss of its ability to self‐interact.     

Two new compounds from Coriaria nepalensis

Two new compounds,corialins A(1) and B(2) were isolated from Coriaria nepalensis Wall.These new compounds were established as 7-hydroxy-3-[2,3-acetonide-(3-methylbutane)]coumarin(1) and 3-O-β-D-glucopyranosyl-3,4,5-trihydroxy-1-(3- methyl-2-butenyl)-benzene(2),on the basis of 1D and 2D NMR techniques.     

Synthesis, Crystal Structure, and Herbicidal Activities of 2-Cyanoacrylates Containing 1,3,4-Thiadiazole Moieties

Three series of novel 2‐cyanoacrylates 7a – 7f , 9a – 9f , 10a – 10f containing 1,3,4‐thiadiazole ring moieties were synthesized as herbicidal inhibitors of photosystem II (PS II) electron transportation. Their structures were clearly verified by ¹H NMR, ¹³C NMR, elemental analysis (or HRMS analysis) and single‐crystal X‐ray diffraction analysis. Bioassay showed that a suitable group at the 3‐position of acrylates was essential for high herbicidal activity. In particular, compound 7e showed the best herbicidal activities and gave 100% inhibitory activity against rape and amaranth pigweed at a dose of 1.5 kg/ha. Introduction of substituent with higher polarity such as sulfinyl or sulfonyl to the 5‐position of 1,3,4‐thiadiazole decreased herbicidal activities.     

Off-on-off luminescent switching of a dye containing imidazo[4,5-f][1,10]phenanthroline

A new acid-base fluorescent switch containing both imidazo[4,5-f][1,10]-phenanthroline and triphenylamine groups has been synthesized.Its fluorescence emissions and absorptions can be reversibiy changed through protonation/deprotonation of imidazole and amine moiety by controlling the intramolecular charge transfer(ICT) process,leading to off-on-off fluorescent molecular switching.     

High performance liquid chromatography with immobilized Ru(bpy)_3~(2+)-KMnO_4 chemiluminescence detection and its application in metabolism of repaglinide in pig liver microsomes

A novel high performance liquid chromatography-chemiluminescence（HPLC-CL） method for investigation of in vitro metabolism of repaglinide in pig liver microsomes with microdialysis sampling technique was developed.The chromatographic separation was performed on a Hypersil BDS-C18 column with an isocratic mobile phase consisting of methanol and 0.01 mol/L KH₂PO₄（pH 3.0）（volume ratio 75:25） at a flow rate of 1.0 mL/min.The detection was based on the chemiluminescence reaction of repaglinide with acidic potassium permanganate（KMnO₄） and tris（2,2’-bipyridyl）ruthenium（Ⅲ）(Ru（bpy）₃³⁺),which was immobilized on the cationic ion-exchange resin for obtaining high sensitivity and reducing consumption of expensive reagent.     

胶原／磷酰胆碱复合膜的制备和性能研究

用静电纺丝-溶液浇注法制备胶原／聚2-甲基丙烯酰氧基乙基磷酰胆碱（pMPC）双层复合膜。用核磁共振波谱仪（NMR）、傅里叶变换红外光谱仪（FTIR）、热重分析仪（TG／DTG）分别表征了pMPC的化学结构、胶原／pMPC分子间的相互作用和共混相容性,用环境扫描电子显微镜（SEM）、X射线光电子能谱仪（XPS）、静态接触...     

固体进样-冷原子吸收法测定食用明胶中的微量汞

样品直接置于石英舟中,在高纯氧气氛中燃烧,释放出的汞与齐化管中的金形成金汞齐,于900℃加热释放出汞蒸气,用冷原子吸收法测定汞的含量。方法的检出限为0.003 ng,测定结果的相对标准偏差为1.13%(n=6),加标回收率为90.5%~97.0%,并用标准样品对方法进行了确证。该方法具有良好的精密度与准确度,适用于明胶中微量汞的测定。