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991.
Zhi-Rong Tan Yao Chen Gan Zhou Shan Cao Xiang-Dong Peng Yi-Cheng Wang Xiu-Juan Peng Wei Zhang Hong-Hao Zhou 《Chromatographia》2010,72(11-12):1107-1113
A sensitive and specific liquid chromatography–electrospray ionization-tandem mass spectrometry method has been developed and validated for the identification and quantification of ursolic acid in human plasma using glycyrrhetic acid as an internal standard. The method involves extraction with methyl tert-butyl ether. The analyte was separated on a C18 column and analyzed in multiple reaction monitoring mode with a negative electrospray ionization interface using the [M–H]? ions, m/z 455.4 for ursolic acid and m/z 469.5 → m/z 425.5 for glycyrrhetic acid. The method was validated over the concentration range of 0.86–110.0 μg L?1. The intra- and inter-day precisions were less than 13.53% relative standard deviation (RSD) and the accuracy was within ?4.76% in terms of relative error (RE). The lower limit of quantification was 0.86 μg L?1 with acceptable precision and accuracy. There were almost no matrix effects. Recovery of ursolic acid from spiked drug-free plasma was higher than 68%. The method was used to study the pharmacokinetic profile of ursolic acid in human plasma after oral administration of Jieyu capsules. 相似文献
992.
Bin Guo Zhiqiang Huang Meiling Wang Xiaoying Wang Ying Zhang Bo Chen Yongjun Li Hongfei Yan Shouzhuo Yao 《Journal of chromatography. A》2010,1217(29):4796-4807
A fast and flexible multi-residue procedure for effective extraction of benzimidazole fungicides and the related transformation products in various raw agricultural commodities is developed for direct and simultaneous analysis by liquid chromatography–tandem mass spectrometry (LC–MS/MS). The new sample preparation method, introduced to allow direct extraction of the labile fungicides as the intact forms in complex matrices, is achieved using a conservative homogenizing extraction and multifunction adsorption cleanup (CHEMAC), which basically involves salting-out partitioning/extraction with acetate-buffered acetonitrile at low-temperature and sequential rapid solid-phase dispersive cleanup with a ternary sorbent mixture. The CHEMAC procedure was optimized and further modified by incorporating several pretreatment variables influencing sample stability and process efficiency, such as pH, temperature, salt and sorbent utilized. By using CHEMAC, a noteworthy improvement in extraction recoveries was obtained for the problematic fungicides, while no significant differential matrix effects were detected on the LC–MS/MS analysis in all 9 matrices. The in-source fragmentation of benomyl occurred but caused no cross-talk interference in multi-component analysis. Thus the CHEMAC-based LC–MS/MS strategy can serve as an attractive approach to satisfactory overall process efficiencies (70–92%) with acceptable repeatability (relative standard deviations below 16%) for all the analyte–matrix combinations. Mean accuracies were obtained within the range of 70–110% at fortified levels of 1–500 ng/g, with intra-day and inter-day variations less than 15 and 20%, respectively. The successful practical application of the proposed method to real samples has also been demonstrated. 相似文献
993.
<正>High density polyethylene(HDPE)/polyethylene-block-poly(ethylene glycol)(PE-b-PEG) blend porous membranes were prepared via thermally induced phase separation(TIPS) process using diphenyl ether(DPE) as diluent.The phase diagrams of HDPE/PE-b-PEG/DPE systems were determined by optical microscopy and differential scanning calorimetry(DSC).By varying the content of PE-b-PEG,the effects of PE-b-PEG copolymer on morphology and crystalline structure of membranes were studied by scanning electron microscopy(SEM) and wide angle X-ray diffraction(WAXD). The chemical compositions of whole membranes and surface layers were characterized by elementary analysis,Fourier transform infrared spectroscopy-attenuated total reflection(FTIR-ATR) and X-ray photoelectron spectroscopy(XPS).Water contact angle,static protein adsorption and water flux experiments were used to evaluate the hydrophilicity,antifouling and water permeation properties of the membranes.It was found that the addition of PE-b-PEG increased the pore size of the obtained blend membranes.In the investigated range of PE-b-PEG content,the PEG blocks could not aggregate into obviously separated domains in membrane matrix.More importantly,PE-b-PEG could not only be retained stably in the membrane matrix during membrane formation,but also enrich at the membrane surface layer.Such stability and surface enrichment of PE-b-PEG endowed the blend membranes with improved hydrophilicity,protein absorption resistance and water permeation properties,which would be substantially beneficial to HDPE membranes for water treatment application. 相似文献
994.
<正>Zein/chitosan composite fibrous membranes were fabricated from aqueous ethanol solutions by electrospinning. Poly(vinyl pyrrolidone)(PVP) was introduced to facilitate the electrospinning process of zein/chitosan composites.The asspun zein/chitosan/PVP composite fibrous membranes were characterized by scanning electron microscopy(SEM) and tensile tests.SEM images indicated that increasing zein and PVP concentrations led to an increase in average diameters of the composite fibers.In order to improve stability in wet stage and mechanical properties,the composite fibrous membranes were crosslinked by hexamethylene diisocyanate(HDI).The crosslinked composite fibrous membranes showed slight morphological change after immersion in water for 24 h.Mechanical tests revealed that tensile strength and elongation at break of the composite fibrous membranes were increased after crosslinking,whereas Young's modulus was decreased. 相似文献
995.
采用脉冲激光烧蚀技术(PLA)在n型Si(100)单晶衬底上制备Tb-Si纳米颗粒。原子力显微镜(AFM)观察样品的表面形貌,发现样品表面是均匀分布的纳米颗粒,颗粒尺寸在10~20 nm之间,分布密度大约为6×1010/cm2。光电子能谱(XPS)及高分辨透射电镜(HRTEM)分析表明,纳米尺度的单晶硅化物颗粒的主要成分为Tb-Si及少量Tb-Si-O结构。室温下以荧光为激发光对样品的光致发光(photoluminescence)性能进行测试,结果表明样品在可见光区具有较强的发光现象,主要有4个发光峰,分别位于485,545,585和620 nm附近,这些发光峰主要由Tb3+中电子在不同能级之间的跃迁造成。 相似文献
996.
苯丙炔酸低聚物的合成及性能 总被引:1,自引:0,他引:1
极性-共轭双取代乙炔-苯丙炔酸在Pd(PPh3)2Cl2催化下直接通过易位催化机理聚合为低聚物.单体苯丙炔酸由两步制得,先通过液溴和肉桂酸的加成反应得到二溴代苯丙酸,然后消去两分子溴化氢得到单体.通过红外光谱(IR)、核磁共振(NMR)对单体及低聚物的结构进行了表征.凝胶渗透色谱(GPC)结果显示,聚合反应以甲苯作溶剂,75℃下效果最好,产率中等.这种共轭低聚物可以溶于四氢呋喃(THF)等极性溶剂,TGA结果表明低聚物热稳定性高.紫外可见吸收光谱(UV-Vis)显示,由于聚合后共轭主链大大增长,苯丙炔酸低聚物骨架上电子的跃迁使得低聚物的四氢呋喃溶液在波长高于310 nm光谱的区域中有吸收.荧光光谱(FS)显示,低聚物的四氢呋喃溶液在342 nm激发光下发蓝光,420 nm处有特征荧光发射峰. 相似文献
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