杏鲍菇多糖的提取及含量测定

采用苯酚-硫酸分光光度法对杏鲍菇中多糖含量进行了测定。测定波长485 nm,多糖换算因子f=1.57,在5.00~70.00μg/mL范围内吸光度与被测物含量呈良好的线性关系,相关系数r=0.999 8,方法的回收率在98.6%~102.3%之间,相对标准偏差RSD在2.01%~2.94%之间。测定结果表明,杏鲍菇中含有丰富的多糖。该法简便、准确、重现性好,可作为杏鲍菇多糖含量的测定方法。     

车前子多糖的测定方法研究

建立了一种准确测定车前子中多糖的方法。采用苯酚-硫酸法测定车前子中多糖量,以木糖作为标准对照物,检测波长480 nm。实验结果表明,车前子中多糖平均值为9.04%,平均加标回收率为98.2%,RSD=1.7%(n=6)。此测定方法适用于车前子多糖含量的测定,也可为其他戊糖含量高的多糖测定提供参考。     

荧光光谱法测定灵芝多糖的含量

采用苯酚-硫酸法建立了灵芝多糖的荧光光谱测定方法。当葡萄糖浓度为20～100μg.mL-1时,λem=518nm处荧光强度与葡萄糖浓度有良好的线性关系,相关系数为0.9994,检出限为6.35μg.mL-1。用拟定的方法对9种灵芝样品进行了测定,其多糖含量在0.712%～2.548%之间,与《药典》法测定结果一致。加标平均回收率为99.82%,相对标准偏差为3.46%。该法结果稳定、重复性好,可用于天然产物中多糖含量的分析。     

青钱柳中多糖的测定

建立了一种测定青钱柳中多糖的方法. 青钱柳样经80%乙醇回流除去单糖、双糖、低聚糖、多酚、氨基酸等杂质后用水提取, 得青钱柳多糖, 其含量采用蒽酮-硫酸法比色测定, 用精制青钱柳多糖测得青钱柳多糖对葡萄糖的换算因子. 采用该方法测定简便可行, 供试液在8 h内显色稳定, 重现性较好, 平均回收率为100.8%, RSD为1.9% (n=3). 所测江西修水青钱柳中多糖含量为4.39%.     

苯酚-硫酸法测定西宁地区地木耳中多糖含量

建立地木耳中多糖的含量测定方法。采用苯酚-硫酸法,以葡萄糖为标准品,在490nm测定多糖的含量。葡萄糖在0.005~0.045mg/mL范围内呈良好线性关系,回归方程A=0.0109ρ-0.0033,R2=0.9996,平均回收率99.8%,RSD为3.4%。     

光度法测定新疆阿魏中多糖的含量

采用苯酚-硫酸光度法对新疆阿魏中多糖含量进行了测定.测定波长485nm,多糖换算因子f=3.179,在10.0～70.0 mg·L-1范围内吸光度与被测物含量呈线性关系,方法的回收率在98.6%～102.2%之间.方法的相对标准偏差(n=5)为0.20%.     

各生长期黄芪中黄芪多糖及微量元素的含量测定

采用水提醇沉法制备多糖粗提物，采用苯酚￣硫酸比色法测定多糖含量，原子吸收法测定微量元素的含量。结果表明：在不同时期采集的栽培品及野生品中，以１０月底１１月初、５月初的栽培品多糖及Ｃｕ、Ｚｎ、Ｍｎ、Ｆｅ含量最高。     

ICP-AES法测定锰铁中的砷、锡、锑

探讨采用ICP-AES法、利用同一母液、一次实现锰铁中的As、Sn、Sb 3种微量元素成分测定的方法.通过试验确定了溶样方法、仪器最佳工作参数、合适的分析谱线等.该法测定As、Sn、Sb含量的相对标准偏差均小于10%(n=10),线性相关系数大于0.9999,加标回收率为98%～102%.该方法缩短了分析周期,精密度、准确度满足检测要求.     

不同月份栽培藏木香微量元素的含量测定及动态分析

采用火焰原子吸收光谱法对不同月份栽培藏木香中Cu、Zn、Fe、Mn、Ca、K、Mg和Na8种微量元素进行了分析测定。结果表明,在选定的测定条件下,栽培藏木香中各元素间相互干扰小,对测定无明显影响。方法的标准曲线线性关系良好(r=0.997 3~0.999 9),方法回收率(n=7)在97.5%~100.3%之间,RSD值(n=7)在1.16%~2.76%之间。栽培藏木香中K、Ca、Mg含量较高且不同月份微量元素含量有所不同,其中Zn、Cu、Mn含量基本稳定;K、Na、Ca、Mg、Fe等元素含量呈现较大幅度的变化趋势。研究结果为合理利用藏木香资源提供了可靠依据。     

微波消解-ICP-AES同时测定宠物食品中的钾、钠、钙、磷

研究了经微波消解宠物食品,采用电感耦合等离子体发射光谱法(ICP-AES)快速测定其中的K、Na、Ca、P 4种微量元素含量的方法。该法不需添加掩蔽剂,很好地解决了使用掩蔽剂带来的偏差。测定样品中K、Na、Ca、P4种元素的相对标准偏差分别为1.68%、4.17%、0.82%、1.44%(n=6),回收率为98.6%~100.1%。该法适用于宠物食品的大批量快速检测。     

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。     

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.

     

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.     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

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^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。