Comparative analysis of the main active components and hypoglycemic effects after the compatibility of Scutellariae Radix and Coptidis Rhizoma

In this study, a rapid and highly sensitive ultra high performance liquid chromatography with triple quadrupole mass spectrometry method with the mobile phase of acetonitrile and 0.1% aqueous formic acid was established and successfully applied to comparatively analyze main active components after their compatibility. Besides, the effects of Scutellariae Radix, Coptidis Rhizoma and combined extracts on type 2 diabetic rats induced by high‐fat diet along with low dose of streptozocin were investigated. Under the optimized chromatographic conditions, good separation of seven target components was achieved within 12 min. All calibration curves exhibited good linearity (R² ≥ 0.999). The relative standard deviation of precision, repeatability and stability varied from 0.69 to 2.23, 0.98 to 2.56, and 0.92 to 2.57%, respectively. The recovery ranged from 91.11 to 105.35%. The contents of seven active components were notably reduced after compatibility; however, the hypoglycemic effect of combined extracts was stronger than single drug by decreasing the activities of fructose‐1,6‐bisphosphatase, glucose 6‐phosphatase, phosphoenolpyruvate carboxykinase and increasing the activities of glucokinase, phosphofructokinase, pyruvate kinase. Accordingly, the established analytical method was accurate and sensitive enough for quantitative evaluation of seven investigated compounds. Moreover, the combined extract had definite effects on type 2 diabetes through multiple components against multiple targets.     

Serum pharmacochemistry combined with multiple data processing approach to screen the bioactive components and their metabolites in Mutan Cortex by ultra‐performance liquid chromatography tandem mass spectrometry

Root cortex of Paeonia suffruticosa Andrews (Paeoniaceae), known as Moutan Cortex (MC), is known to have anti‐allergic and anti‐inflammatory properties. However, the constituents absorbed into blood after oral administration of MC remain unknown. A sensitive and rapid method by ultra‐high‐pressure liquid chromatography–electrospray ionization–quadrupole‐time‐of‐flight mass spectrometry (UPLC‐ESI‐Q‐TOF‐MS) technology and the MetaboLynx^TM software combined with multiple data processing approach (Mdpa) was established to investigate the absorbed constituents in rats after oral administration of MC, providing unique high‐throughput capabilities for drug metabolism study. A hyphenated electrospray ionization and quadrupole‐time‐of‐flight analyzer was used for the determination of accurate mass of the fragment ion in negative mode, with excellent MS mass accuracy and enhanced data acquisition. This rapid automated analysis method was successfully applied for screening and identification of the constituents absorbed and metabolized studies of MC after oral administration to rats. A total of 46 peaks were obtained from MC, 41 of which were tentatively characterized. In the VIP‐plot of orthogonal partial least‐squares discriminant analysis, 23 interesting ions in serum samples were extracted, and 16 parent components and seven metabolites were detected in vivo. The integrative serum pharmacochemistry technique, UPLC‐ESI‐Q‐TOF‐MS, and Mdpa method were successfully applied for rapid discovery of multiple components from MC. Copyright © 2013 John Wiley & Sons, Ltd.     

催化裂解-金汞齐富集-冷原子吸收光谱仪测定土壤样品中总汞含量

为建立采用催化裂解-金汞齐富集-冷原子吸收光谱仪即直接测汞仪测定土壤样品中汞含量的方法,本研究配制汞总量为0~2 ng、0~15 ng和25~1023 ng的三种不同汞浓度系列的标准工作曲线,选取9个土壤样品,3种国家土壤有证标准物质,同一样品分别进行6组平行测定,并抽取3个土壤样品进行3种不同浓度加标回收试验,以对其方法精密度和准确度进行论证。 结果显示：仪器信号值与Hg总量之间均呈良好的线性关系。根据仪器多次测定空白数据结果,按照称样量0.1 g计算,方法最小检出量为0.09 ng/g;平行测定结果相对标准偏差均小于10%,土壤标准物质测定值与标准物质标准参考值均相符,不同浓度的加标回收率范围为78.4%～92.7%。结果表明催化裂解-金汞齐富集-冷原子吸收光谱仪,可用于批量土壤样品中汞含量的快速测定分析,方法的精密度和准确度可满足测定分析要求,且实验过程中无需前处理消煮,操作方便、快速高效。     

增敏剂改进超级微波消解-电感耦合等离子体质谱(ICP-MS)法测定食品中硒元素

合适比例增敏剂会对超级微波消解-电感耦合等离子体质谱法(ICP-MS)测定食品中硒元素含量具有一定的优化效果。本文采用超级微波消解仪对1.0 g食品样品进行全消解,采用碰撞池模式规避质谱干扰,内标校正非质谱干扰,选择甲醇、乙醇、乙酸、异丙醇、丙三醇作为增敏剂,并调整测试过程中的添加比例,用电感耦合等离子体质谱法测定。结果表明：2%异丙醇存在时硒元素各同位素响应值最高,其中78Se具有低至0.0003 mg·kg-1的方法检出限;用以上方法对食品标准物质（GSB-8、GSB-9、GSB-24、GSB-30）及实际样品进行分析,标准物质测定值均在其认定值及不确定度范围内,相对误差小于-5.4%;实际样品测定值的相对标准偏差（n=7,RSD）为0.3~1.7%,加标回收率为99.2~105%。本方法操作简便,精密度好,准确度高,可以作为各类食品样品中硒含量测试方法。     

Co-N-C体系催化α-芳香醇氨氧化直接制备α-芳香腈

以Co(NO_3)_2·6H_2O和1-丁基-3-甲基咪唑氢溴酸盐为前驱体,Vulcan XC72R为载体,采用浸渍法制备负载型Co-N-C催化剂,使用XRD、 XPS、 HRTEM等手段对其结构进行了表征.以α-芳香醇催化氨氧化合成α-芳香腈为考察对象,对其催化性能进行了评价.例如,在O_2压力为0.5 MPa,反应温度为120℃,反应时间为20 h的条件下,以Co-N-C/700为催化剂,NH_3(aq)为氨源,在催化苯甲醇合成苯甲腈反应中,苯甲醇转化率可达100%,产物苯甲腈选择性为100%.     

同位素示踪法的开创者——赫维西

19世纪末20世纪初是物理化学和生物化学发展的重要时期,同位素示踪法在一系列示踪剂实验方面取得了许多成就。瑞士籍匈牙利裔化学家乔治·德·赫维西(1885—1966)将示踪技术应用到生物学领域,他有关同位素示踪法的发明也使其获得了1943年诺贝尔化学奖。本文对赫维西生平及学术成长历程进行介绍,反映了赫维西的成长与欧洲当时的诸多科学家之间的学术往来是不可分割的。     

200℃偶极发射换能器研究

高温偶极子发射换能器是200℃高温多极子阵列声波测井仪器研发需要攻克的主要核心关键技术问题之一。针对这一问题,该文从材料选型和工艺改良两个方面开展技术攻关,研发了耐温达200℃偶极子发射换能器,样机耐温性能测试表明其能够在200℃下连续工作12 h而不损坏,声性能测试样机最大发射电压响应为124 dB,具有与现用换能器相当的辐射性能,样机尺寸及工作频率与现用换能器几乎完全一致,可以方便地对现用仪器进行升级。目前搭载该样机的仪器已经通过孤古8实验井测试,并在新疆顺北油田现场近9000 m井下取得高质量数据,达到设计目的。该文为开展更高温换能器研发提供了详细的研究思路。     

超声辅助电镀的仿真与实验*

为了提高镀层的表面质量,提出了一种超声辅助电镀的方法。超声的空化与搅拌作用可以影响电镀的电沉积过程。设计了合理的换能器结构,并搭建了超声辅助电镀装置。通过对模型进行压电声学场与电镀场耦合仿真分析,结果表明：在硫酸铜电解液,镀铜时间60s,电压300V条件下,进行超声辅助电镀,镀层厚度分布均匀,镀层中部电流密度分布均匀,边缘最大电流密度是未加超声的2倍左右 。基于仿真结果,进行相同的实验测试,结果表明：超声辅助电镀可以提高镀层的均匀性,减少铜颗粒表面的杂质,提高表面的光洁度。阴极样品距离换能器头部位置在60mm左右,镀层质量良好。