Preparation of benzene adsorption materials using waste activated alumina

A new type of benzene adsorption material was prepared by using the airtight heat treatment method. This method can directly transform the organic impurities of the activated alumina waste into carbon with adsorption capability. The microstructure and carbon content of materials were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), BET (Brunauer Emmett Teller) surface area analysis and elemental analysis. The influences of heat treatment temperature on the properties of the composite materials were discussed. The benzene adsorption capability of the material was investigated. The experimental results show that the optimal heat treatment process condition is airtight heating at 400°C for 2 h. The resulting sample has carbon mass fraction of 3.57%, specific surface area of 234.70m²/g, pore volume of 0.41m³/g, and average pore size of 6.59 nm. The samples show excellent benzene adsorption capability with an adsorption rate of 21.80%.     

引阳素胶囊中淫羊藿苷的含量测定

目的建立引阳素胶囊中淫羊藿苷的高效液相色谱(HPLC)含量测定方法。方法采用HPLC法。色谱柱Li-chrospher C18(4.6 mm×250 mm,5μm),C18保护柱;流动相为乙腈-20 g/L冰醋酸水溶液(30∶70);检测波长270 nm;流速1.0 mL/min;柱温为室温;进样量10μL。样品加50%(体积分数)乙醇超声提取,浸提液过0.45μm滤膜后测定。结果淫羊藿苷线性范围为10.0-60.0 mg/L,回归方程为C=2.042×10-5A+0.554,r=0.9993,平均回收率为99.8%,RSD为0.65%。结论本法用于引阳素胶囊中淫羊藿苷的含量测定时简便快捷、准确。     

油菜(Brassica campestris L.)秸秆生物炭对Cr(Ⅵ)的吸附研究

研究了油菜秸秆生物炭对Cr(Ⅵ)的吸附性能、影响因素及吸附动力学和吸附热力学.实验结果表明:该生物炭对Cr(Ⅵ)的吸附受pH、时间、Cr(Ⅵ)初始浓度等因素的影响.其中:pH是影响其吸附性能的重要因子.溶液中Cr(VI)的去除率随溶液pH值降低而升高,在pH值为2.0时达到最大98.87%.油菜秸秆生物炭对Cr(Ⅵ)的吸附符合准二级吸附速率方程,吸附等温线与Langmuir等温方程拟合较好,20℃、25℃、30℃和35℃下的最大吸附量分别为5.96、6.62、7.49和8.59mg/g.吸附量随温度的升高而增加,说明油菜秸秆生物炭对Cr(Ⅵ)的吸附机理主要是吸热的化学吸附.     

泡沫混凝土气孔结构数学表征及其分析

为分析泡沫混凝土孔结构表征参数之间的关系和气孔结构特点,建立了紧密堆积模型和非紧密堆积模型,基于不同的理论模型推导了孔结构主要参数包括孔隙率、气孔内表面积、气孔壁厚度的计算公式,分析各参数之间的关系;通过实测泡沫混凝土的孔结构参数,验证了计算公式的可行性,并将计算公式应用于泡沫混凝土孔结构特征分析. 研究结果表明:当容重等级小于1 000 kg/m3时,泡沫混凝土形成的气孔结构为紧密堆积型结构,气孔壁厚计算结果与统计结果偏差在12%以内,验证了紧密堆积型结构计算公式的可行性;当容重等级大于或等于1 000 kg/m3时,泡沫混凝土形成的气孔结构为非紧密堆积型结构,气孔壁厚计算结果与统计结果偏差在3%以内,验证了非紧密堆积型结构计算公式的可行性;在相同容重下,气孔壁厚度随气孔直径的增大而增大,随孔隙率的增大而减小;1 m3泡沫混凝土的气孔内表面积可达到3 000 m2以上,气孔壁厚可低至60 μm以下,泡沫混凝土具有多孔薄壁、小体积物料与大体积的气孔空气共存于一体、小体积物料以巨大的面积暴露在气孔的气体之中的结构特征.      

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

Objective High performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS) methods were developed for the determination of ganciclovir and its related substances. Methods A Hypersil ODS2 column (4.6mm×250mm, 5μm) was used with a mobile phase of 0.02M potassium 1.0mL/min, and UV detector set at 254nm was used for monitoring the eluents. Results The method was simple, rapid, selective and capable of separating all related substances at trace level with a detection limit of 0.04μg/mL. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 10.2-153.0μg/mL with r=0.9998. The percentage recoveries ranged from 96.7% to 101.6%, and RSD was 1.24%-1.96% (n=5). Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir. For identification of related substances, LC/MS was used. The mainly related substances of ganciclovir active pharmaceutical ingredients (API) were determined as guanine, (1, 3-dioxolan-4-yl) methyl acetate, and diacetyl guanine.     

P123模板氧化铝介孔材料制备及性能

以PEO-PPO-PEO三嵌段共聚物P123为模板剂,异丙醇铝为铝源,以水为介质通过水热合成技术合成出了氧化铝介孔材料.通过调节P123的用量,得到了孔道结构呈蠕虫状、比表面积较大、平均孔径在15 nm左右、孔容在1.0 cm3/g以上的氧化铝介孔材料;但其孔径分布稍宽.实验结果证明,加入适当量的模板剂能够明显改善氧化铝介孔材料的孔结构特征.     

Analysis and determination of diterpenoids in unprocessed and processed Euphorbia lathyris seeds by HPLC-ESI-MS

Euphorbia lathyris （Caper spurge） is a toxic and potent Chinese materia medica （T/PCMM）. This study sought a method for identifying five diterpenoids （Euphorbia factors LI-L3, L7a, and Ls） with the spectra of UV and mass, quantifying three diterpenoids L1, L2, and L8 in crude extracts of unprocessed and processed E. lathyris seeds by liquid chromatography/ electrospray ionization mass spectrometry （LC-ESI-MS）. The analysis was achieved on an Agilent Eclipse XDB-C18 column （4.6 mm× 150mm i.d., 5 μm） with an isocratic elution with a mobile phase consisting of water and acetonitrile at a flow rate of 0.25 mL/min at column temperature of 30 ℃ and UV detection was set at 272 nm. An ESI source was used with a positive ionization mode. The calibration curve was linear in the ranges of 9.9-79 μg/mL for Euphorbia factor Lb 3.8-30.5μg/mL for Euphorbia factor L2, and 1.0-20.6 μg/mL for Euphorbia factor LB. The average recoveries （n=6） of three diterpenoids were 98.39%, 91.10% and 96.94%, respectively, with RSD of 2.5%, 2.4% and 2.1%, respectively. The contents of the three diterpenoids in processed E. lathyris seeds were 3.435, 1.367 and 0.286 mg/g, respectively, which decreased more sharply than those in unprocessed E. lathyris seeds which were 4.915, 1.944 and 0.425 mg/g, respectively. The method is simple, accurate, reliable and reproducible, and it can be applied to control the quality of unprocessed and processed E. lathyris seeds.     

Simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture by high performance liquid chromatography

A reversed phase high performance liquid chromatography （HPLC） method was established for the simultaneous determination of 12, 13-dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture. A Grace Apollo Cl8 column （250 mm × 4.6 mm, 5 μm） was used as the stationary phase and the mobile phase was composed of acetonitrile and aqueous phosphoric acid （0.2%, v/v）. Gradient elution was carried out at the flow rate of 1.0 mL/min and the column temperature was 30 ℃. An ultraviolet （UV） detector was used with a selected wavelength of 240 nm. Calibration curves were linear within the concentration range of 4.6-45.75 μg/mL for 12, 13-dihydroxyeuparin （r〉0.9999） and 106.9-1068.9μg/mL for glycyrrhizic acid （r〉0.9999）, respectively. Recoveries were 102.18% for 12, 13-dihydroxyeuparin and 101.17% for glycyrrhizic acid. The method developed could be applied to the simultaneous determination of 12, 13- dihydroxyeuparin and glycyrrhizic acid in Yanyanfang mixture.     

DETERMINING THE CONTENT OF JASMINODIN IN MEI RONGCAPSULE WITH THIN LAYER CHROMATOGRAPHY

Cardenia Jasminoides may bring about the ef-fects of laxative, being antipyretic, diuresis detoxi-cation, and anti--inflammation[1J. It has been provedthat the main active component of Cardenia Jas-minodin Eills is the iridoid glycosides representedby Jasminodin['.'J. Recently, with the improvementof people's living conditions in China,Cardenia Jas-minodin Eills has been applied in several kind ofcosmetics and proved to be effective in eliminatingacnes, disinfecting and beautifying the ski…     

EFFECTS OF TOTAL SAPONINS OF PANAX NOTOGINSENG AND LIGUSTRAZINE ON THE PROLIFERATION OF CEREBRAL MICROVASCULAR ENDOTHELIAL CELLS OF RATS

Ｅｎｄｏｔｈｅｌｉａｌｃｅｌｌｓ (ＥＣｓ)ｆｕｎｃｔｉｏｎａｓｔｈｅｂａｒｒｉｅｒｏｆｔｈｅｂｒａｉｎａｎｄｒｅｌａｔｅｔｏｔｈｅｓｅｃｒｅｔｉｏｎｏｆｓｏｍｅｅｎｄｏ ｃｒｉｎｅｓ.Ｔｈｅｉｒｄｙｓｆｕｎｃｔｉｏｎｉｓｃｌｏｓｅｌｙｒｅｌａｔｅｄｔｏｔｈｅｏｃｃｕｒｒｅｎｃｅａｎｄｄｅｖｅｌｏｐｍｅｎｔｏｆｃｅｒｅｂｒａｌｖａｓｃｕｌａｒｄｉｓｅａｓｅｓ[1] .ＤａｍａｇｅｔｏＥＣｓｉｓｔｈｅｆｉｒｓｔｓｉｇｎａｎｄａｂａ ｓｉｃｆａｃｔｏｒｏｆｃｅｒｅｂｒａｌｉｓｃｈｅｍｉａ .Ｔｈｅｒｅｆｏｒｅ ,…     

Thermal Transport in Nanoporous Yttria-Stabilized Zirconia by Molecular Dynamics Simulation

Yttria-stabilized zirconia (YSZ) is widely used as thermal barrier coatings (TBCs) to reduce heat transfer between hot gases and metallic components in gas-turbine engines. Porous structure can generally reduce the lattice thermal conductivity of bulk material, so porous YSZ can be potentially used as TBCs with better thermal performance. In this work, we investigate the thermal conductivity of nanoporous YSZ using the nonequilibrium molecular dynamics (NEMD) simulation, and comprehensively discuss the effects of cross-sectional area, pore size, structure length, porosity, Y₂O₃ concentration and temperature on the thermal conductivity. To compare with the results of the NEMD simulation, we solve the heat diffusion equation and the gray Boltzmann transport equation (BTE) to calculate the thermal conductivity of the same porous structure. From the results, we find that the thermal conductivity of YSZ has a weak dependence on the structure length at the length range from 10 to 26 nm, which indicates that the majority of heat carriers have very short mean free path (MFP) but there exists small percentage (about 3%) of phonons with longer MFP (larger than 10 nm) contributing to the thermal conductivity. The thermal conductivity predicted by NEMD simulation is smaller than that of solving heat diffusion equation (diffusive limit) with the same porous structure. It shows that the presence of pores affects phonon scattering and further affects the thermal conductivity of nanoporous YSZ. The results agree well with the solution of gray BTE with a average MFP of 0.6 nm. The thermal conductivity of nanoporous YSZ weakly depends on the Y₂O₃ concentration and temperature, which shows the phonons with very short MFP play the major contribution to the thermal conductivity. The results help to better understand the heat transfer in porous YSZ structure and develop better TBCs.     

治带片中苦参碱及氧化苦参碱的HPLC法测定

目的建立治带片中苦参碱及氧化苦参碱的高效液相色谱(HPLC)测定方法。方法色谱柱:Lichrospher-NH2(4.6 mm×250 mm,5μm),C18保护柱;流动相:乙腈-无水乙醇-0.5 mol/L磷酸水溶液(80∶10∶10);检测波长212 nm;流速1.0 mL/min;柱温:室温;进样量20μL。结果苦参碱和氧化苦参碱线性范围均为1.0-10.0μg/mL,回归方程苦参碱为:C=1.201×10-4A+0.161,r=0.9992;氧化苦参碱为:C=1.366×10-4A+0.221,r=0.9996,平均回收率分别为99.9%和99.4%,RSD分别为1.48%和4.33%。结论本法简便快捷,结果准确,可用于该制剂的质量控制。     

“鸟枪”蛋白组学技术鉴定牙龈卟啉单胞菌47A-1亚型外膜蛋白

目的利用shotgun(鸟枪)蛋白质组学策略鉴定牙龈卟啉单胞菌(Porphyromonas gingivalis,P.g)亚型47A-1外膜蛋白,深化P.g外膜蛋白的蛋白质组学研究,为进一步研究P.g外膜蛋白的致病性奠定基础。方法提取P.g47A-1外膜蛋白,SDS-PAGE电泳分离蛋白,胶内酶解为多肽混合物,应用毛细管高效液相色谱加串联质谱分析,SEQUEST程序进行数据库搜索并鉴定蛋白。结果用考马斯亮蓝法染色凝胶分离的蛋白,发现P.g47A-1蛋白条带主要在14.3~97 ku之间。酶解的肽段经毛细管高效液相色谱分离,得到肽段水平的总离子流图,分析肽段序列后发现P.g47A-1蛋白有623个唯一肽段,鉴定出136种蛋白,包括了51种已知蛋白,85种未知蛋白。结论 Shotgun技术可分析出P.g47A-1大量未知蛋白,尤其是丰度低、疏水性强的外膜蛋白,优于二维凝胶电泳(two dimensional gelelectrophoresis,2-DE)等传统蛋白质组学方法,为进一步研究P.g外膜蛋白的致病性奠定了基础。     

RP-HPLC method for the simultaneous determination of daidzein,genistein and formonetin in Solanum Lyratum Thunb

A rapid method for the simultaneous determination of daidzein, genistein and formonetin in solanum Lyratum Thunb by high performance liquid chromatography (HPLC) was developed. Separation was achieved on a Diamonsil C18 column (250 mm×4.6 mm, 5 μm) with isocratic elution, using a mobile phase of methanol-tetrahydrofuran-water (44∶3∶53, v/v). The wavelength was set at 260 nm and column was maintained at 35 ℃. The linear ranges of daidzein, genistein and formonetin were 1.0-40.0, 0.1-4.0 and 0.1-4.0 μg/mL, respectively. The average recoveries were between 98.4% and 101.3%. This method could be used for the quality control of Solanum lyratum Thunb due to its simplification, reliability, rapidity and excellent precision.     

肺癌nm23、c-erbB-2基因表达及其临床意义

为探讨ｎｍ２３、ｃ－ｅｒｂＢ－２基因在评估肺癌生物学行为及预后中的作用，应用免疫组化ＡＢＣ法检测了４１例肺癌及３０例癌分组织中ｎｍ２３及ｃ－ｅｒｂＢ－２的表达。结果表明癌组织中ｎｍ２３ｋｃ－ｅｒｂＢ－２表达率显著高于癌旁组织（Ｐ＜０．００１）；两者相关性极强（Ｘ２＝６．６２，Ｐ＜０．０２），且均与癌病理分级、ＴＮＭ分期及肺门和（或）纵隔淋巴结转移（简称分级、分期及转移）呈正相关（Ｐ＜０．００１、０．０１或０．０５）。提示ｎｍ２３及ｃ－ｅｒｂＢ－２基因表达可作为肺癌诊断及预后和生物学行为评估的指标。     

核-壳纳米复合材料制备及含铬重金属处理

采用一步固相法,制备出以富铁空心微珠为基、稀土掺杂纳米铁氧体为壳的核-壳型纳米复合材料.对所制备样品进行X射线衍射（XRD）、扫描电子显微镜（SEM）和磁性能的表征.结果表明成功制备了核-壳型纳米复合材料,样品的晶粒粒径为30 nm,复合材料两相的交换耦合作用增强,剩磁与矫顽力有所改善,提高了复合材料对重金属阳离子的吸附.采用原子吸收光谱法研究了该复合材料对Cr3＋离子的吸附性能,确定了最佳吸附条件.在最佳工艺条件下,该复合材料对含铬重金属的吸附率达到98％以上,有较好的吸附能力,适于推广使用.     

乌头碱在家兔检材中的降解动力学

用高效液相色谱法(High performance liquid chromatography,HPLC)分离测定生物性样品中的乌头碱。对乌头碱在离体生物检材中的降解动力学进行了研究。乌头碱在经不同处理的生物检材(凝血块、肝脏)中以表观二级动力学过程被降解,其降解速率常数K以4%甲醛溶液固定组中为最大(1.5619,0.7728μg/d),其次为95%酒精固定组(0.4891,0.7556μg/d),4℃冰箱放置组中最小(0.06372,0.0393μg/d),亦即中毒检材中乌头碱在冰箱中分解较慢,其次为在酒精固定剂中。从死亡或中毒后一段时间取检材检测,可用建立的动力学方程推算体內乌头碱是否已达中毒量或致死量。     

含增生结节鼠肝谷胱甘肽转硫酶的纯化和性质研究

含增生结节鼠肝GST活性在纯化过程各步均较正常肝明显增高,经DEAE-52和CM-52柱层析分离得阴离子同工酶A-1和A-2以及阳离子同工酶C-1,C-2,C-3和C-4,用等电聚焦电泳测定等电点分别为6.7,6.3,7.4,7.9,8.3和8.6。SDS-PAGE结果显示,含增生结节肝GST在正常大鼠肝GSTYa,Yb和Yc区带相应的位置,出现3条区带,各亚基分子量分别为26,000,27,000和28,600道尔顿,但活性增高明显的C-3和C-4只出现1条相当于Yc亚基的区带。含增生结节肝GST6种同工酶的带电性质及亚基组成与正常肝无明显差别。阳离子同工酶C-3和C-4活性占上柱总活性的70%,说明含增生结节肝GST活性增高以阳离子同工酶为主。     

粉煤灰喷射混凝土孔隙结构的演变特征

为了寻找长期服役的喷射混凝土配合比,采用低场核磁共振技术,研究了不同粉煤灰掺量改性胶凝材喷射混凝土的微观孔隙结构,测定了不同掺量的粉煤灰喷射混凝土在不同养护龄期的微观孔隙结构分布特征及孔隙度.研究结果表明:掺有粉煤灰的喷射混凝土孔隙度随粉煤灰掺量的增加而增大,随龄期的延长总体呈现先减小后趋于平稳的趋势;粉煤灰掺量为10%时孔隙度最小,掺量为0时孔隙度最大;在7 d龄期后,不同粉煤灰掺量的喷射混凝土内部孔隙半径主要在1~80 nm的范围内,该半径范围内的孔隙含量占总孔隙含量的80%,最可几孔半径在12 nm.      

A rapid method for the determination of dopamine in porcine muscle by pre-column derivatization and HPLC with fluorescence detection

A rapid method has been developed based on the sample preparation procedure named as QuEChERS （Quick, Easy, Cheap, Effective, Rugged and Safe）, combined with reversed-phase high performance liquid chromatography with fluorescence detector and C18 column after precolumn derivatization using o-phthalaldehyde and 2-mercaptoethanol to determine dopamine in porcine muscle. Methanol and deionized water （0.1% acetic acid, v/v） with a ratio of 60：40 was used as mobile phase. The flow rate was 0.8 mL/min and dopamine was eluted within 15 min. The linearity range was 0.003-8 μg/mL with r=0.9992. The detection limit for dopamine was 4 μg/kg and the quantification limit was 9 μg/kg. Recovery studies were carried out at 0.1, 0.5 and 1.0 mg/kg fortification levels and the average recoveries obtained ranged from 90.4% to 98.2% with relative standard deviations between 3.5% and 8.1%. The method was found to be suitable for detection of dopamine in animal product tissues at the maximum residue level.