流动注射-分光光度法测定水中氰化物

使用流动注射(FIA)-分光光度法测定水中的氰化物的含量,并与传统分光光度法的分析结果进行比对。实验证明流动注射(FIA)-分光光度法操作简便、线性好,灵敏度、精密度、准确度都能符合分析工作要求。检出限为0.2μg/L,适用于水中微量氰化物的检测。分析频率为每小时30个样品,特别适合大批样品的测定。     

光果甘草乙酸乙酯相对酪氨酸酶的抑制作用

酪氨酸酶是生物体合成黑色素的关键酶,实验以光果甘草为原料,研究其提取物乙酸乙酯相对酪氨酸酶活性的抑制作用及机理.采用L-多巴速率氧化法体外测定光果甘草提取物乙酸乙酯相对酪氨酸酶的抑制活性,并绘制了Lineweaver-Burk双倒数曲线以此判断其抑制类型.结果表明光果甘草提取物乙酸乙酯相半抑制浓度(IC50)为(266.5±1.4)mg/L.对酪氨酸酶抑制机理测定分析的结果表明,光果甘草提取物乙酸乙酯相对酪氨酸酶活性的抑制作用表现为可逆抑制,对酪氨酸酶活性的抑制类型是混合型抑制,抑制常数KI为(182.86±1.43)mg/L,α值为(15.49±0.68)mg/L.可见甘草提取物乙酸乙酯相对酪氨酸酶有较强抑制作用.     

基于竹膜固定酪氨酸酶的L-酪氨酸光度测定法

提出了将酪氨酸酶固定在戊二醛活化的竹膜上制成检测L-酪氨酸的单元,用于L-酪氨酸的光度测定。此方法系基于在pH 7.0的磷酸盐缓冲溶液中酪氨酸酶催化酪氨酸转化为多巴醌,多巴醌进一步与3-甲基-2-苯并噻唑啉酮腙盐酸盐(MBTH)反应生成栗色加合物。此化合物在490 nm波长处有特征吸收峰,并在此波长所测得的吸光度与L-酪氨酸的浓度在5~200μmol·L-1之间呈线性关系,其检出限(3S/N)为2.5μmol·L-1。应用此方法测定了复方氨基酸注射液中L-酪氨酸的含量,所得结果与该药品的标示值一致。     

Bi-NDAC-茜素紫分光光度测定铋

本文报道了在新合成的表面活性剂N,N-二氨丙基十六胺盐酸盐(NDAC)存在下,茜素紫分光光度法测定微量铋。实验结果表明,三胺型阳离子表面活性剂对铋具有富集作用,可以降低铋的检测下限,对茜素紫分光光度法测定微量铋具有较好的增敏作用。实验查明了络合物的吸收光谱,铋-茜素紫二元络合物的最大吸收峰位于579nm,铋-茜素紫-NDAC三元络合物的最大吸收峰位于600nm,红移21nm。经过条件选择实验确定的最佳反应条件是三元络合物在     

卤代查尔酮氨基硫脲席夫碱的合成及生物活性研究

本文合成了一系列卤代查尔酮及其氨基硫脲席夫碱,并考察了所合成化合物的酪氨酸酶抑制活性及抗氧化活性。结果表明,部分化合物具有较好的酪氨酸酶抑制活性,其中3个化合物的抑制活性强于阳性对照曲酸,4-溴代查尔酮氨基硫脲席夫碱(化合物9)表现出最好的抑制活性,其IC50值为2.02μmol/L;部分化合物还具有一定的抗氧化活性。抑制机理研究表明,化合物9属于不可逆抑制剂。优选化合物9进行了分子对接探讨,初步构效关系分析为进一步研究具有酪氨酸酶抑制活性的类似化合物提供了参考。     

光谱法研究夏枯草黄酮对酪氨酸酶的抑制作用

利用紫外-可见光谱法、荧光光谱法和圆二色谱法研究了夏枯草黄酮对酪氨酸酶的抑制作用及抑制机理。结果表明,夏枯草黄酮是一种可逆的竞争型酪氨酸酶抑制剂,且能很快地抑制酪氨酸酶的活性,其半抑制浓度(IC50)为79.25μg/mL,抑制常数(Ki)为130.33μg/mL。荧光光谱显示夏枯草黄酮能显著地增强酪氨酸酶的疏水性。圆二色谱分析表明夏枯草黄酮诱导酪氨酸酶的构象发生了部分改变。     

催化分光光度法测定土壤中痕量碘

化探样品中碘含量的检测常用方法有流动注射-光度法、催化分光光度法、离子色谱法和电感耦合等离子体质谱法等。催化分光光度法测定土壤中痕量碘的方法,准确度和精密度不高。本工作在文献基础上,对方法中样品的分解温度、分解时间、显色波长、显色温度、显色时间、显色酸度、四碱用量、氯胺T用量等各个条件进行了优化试验,确定     

对溴偶氮氯膦流动注射分光光度法测定岩矿中的钪

本文研究了对溴偶氮氯膦与钪在盐酸介质中的显色反应。在波长740nm,络合物的摩尔吸光系数为7.0×10~4,7～18μg Sc_2O_3/25ml符合比尔定律。采用流动注射分光光度法,联合使用微型计算机,测出工作曲线的线性范围为5～45μg Sc_2O_3/25ml,比普通分光光度法扩大1.5倍。应用于测定岩矿中的微量钪,方法快速、准确。     

反相高效液相色谱柱前衍生法测定发酵液中的5-氨基乙酰丙酸

建立了同时检测发酵液中5-氨基乙酰丙酸和甘氨酸的柱前衍生反相高效液相色谱法。使用ZORB-AX SB-AQ型色谱柱(250 mm×4.6 mm i.d.,5μm),以甲醇-50 mmol/L醋酸钠缓冲溶液(pH 6.2)作为流动相梯度洗脱。流速为1 mL/m in,柱温25℃,254 nm波长下检测30 m in。在此条件下,5-氨基乙酰丙酸和甘氨酸在浓度为0.8~23 mmol/L和1.3~66 mmol/L时与色谱峰面积值之间线性关系良好,回归系数均在0.9997以上。发酵液产物的加标回收率在94.9%~104.7%。将检测结果与分光光度法相比,符合较好。测试数据表明,此方法简单、可靠,对于发酵产物的分离效果好。     

流动注射-串联质谱法快速筛选植物提取物对药物代谢酶的抑制潜性

基于流动注射-串联质谱(FI-MS/MS)技术,综合运用微孔板低温孵育、低温样品相分离、六合一进样和多探针同时定量分析,建立了体外快速筛选复杂中草药组分抑制细胞色素P450同工酶活性的新方法。FI-MS/MS新技术不依赖色谱分离,也无需复杂的仪器设备和样品前处理,分析通量大幅提高。采用基质匹配标样和内标法定量,方法的准确度、精密度、灵敏度和线性范围均满足孵育体系中代谢物分析的需要。优化条件下测得各酶动力学参数和对照抑制剂的半抑制率(IC50)均与参考值一致;仅用两抑制剂浓度点即可获得满意的IC50近似值,两点IC50的测试重现性良好。结合两点IC50程序,FI-MS/MS方法成功应用于中药粗提液对人体主要P450酶抑制效应的快速筛选与分类,为多组分体系复杂药代相互作用的研究和评估提供了一种有效手段。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

化学计量中不确定度评定研究进展

测量不确定度是表征合理地赋予被测量之值的分散性的参数。本文针对化学计量不确定度评定基础模型仅适用于线性模型、概率分布为正态分布或缩放位移t分布等局限,介绍了近年来不确定度评定的研究热点:蒙特卡罗方法(Monte Carlo Method,MCM),不确定度评定的来源、评定概念、评估方法及其发展过程,扩大了测量不确定度评定与表示的适用范围。     

微量钙的测定方法研究进展

介绍了1995-2006年期间测定微量和痕量钙的方法,如电感耦合等离子体-原子发射光谱法、原子吸收光谱法以及离子色谱法等的工作原理和特点,并说明了其测定微量钙的应用领域。并对微量钙的测定技术进行了展望(引用文献55篇)。