滇桂艾纳香水溶性多糖BRP-B的分离纯化及止血活性

用蒸馏水溶解滇桂艾纳香浸膏,从中提取多糖,通过膜分离、三氯乙酸法脱蛋白、二乙氨基乙基(DEAE)脱色、SephadexG10、SephadexG50凝胶柱色谱纯化,获得滇桂艾纳香水溶性多糖(BRP-B)。 由凝胶渗透色谱（HPGPC）确定BRP-B为相对分子质量分布均一的多糖,其数均分子量和质均分子量分别为2654和2716 Da。 以血浆复钙时间（PRT）为指标,研究BRP-B的凝血活性,结果显示BRP-B质量浓度为6.25×10-2 g/L时,凝血时间为248.52 s,凝血时间抑制率达22.42%。 小白鼠离体子宫实验结果显示,BRP-B质量浓度为1.67×10-2、1.97×10-2及2.85×10-2 g/L时能明显增加子宫平滑肌的收缩频率。     

正交设计优化木贼多糖的超声提取工艺(英文)

以蒸馏水为溶剂提取,通过单因素实验和正交实验,研究料液比、超声功率、超声提取温度和超声作用时间对木贼多糖提取效果的影响。超声提取法的优化工艺条件为:料液比(g/mL)1∶20,提取温度70℃,超声功率100 W,作用时间50 min。在此条件下,木贼多糖的平均提取率为12.33%,RSD为0.16%。超声波强化提取木贼多糖省时高效。     

高效阴离子交换色谱-脉冲安培检测法分析漏芦多糖中单糖组成

采用高效阴离子交换色谱-脉冲安培检测法(HPAEC-PAD),建立了一种测定漏芦多糖中单糖组成的方法.水提、醇沉法提取粗多糖,Sevage法除蛋白,用2mol·L-1硫酸在100℃水解多糖,以CarboPac PA10色谱柱(2mm×250mm)为分离柱,100 mmol·L-1氢氧化钠溶液为淋洗液,流速为1.0 mL·min-1,脉冲安培检测,总分析时间为6min.测定漏芦多糖中单糖组成为阿拉伯糖、葡萄糖和果糖,其摩尔比为1.55:1.00:2.10;加标回收率为93.0%～107.8%,捡出限为2.8～12.3 μg·L-1.     

固相萃取原子荧光光谱法检测稻米和虾仁中的无机硒

建立了氨水提取、三氯乙酸沉淀蛋白、阳离子交换净化分离,原子荧光光谱检测稻米和虾仁中无机硒的新方法。样品经氨水超声提取,三氯乙酸沉淀蛋白,Cleanert PCX小柱分离,HNO_3-HClO_4消解,HCl还原,原子荧光光谱法进行检测。结果显示,无机硒能被有效提取、分离和检测。方法在(0. 1～4. 0μg/L)浓度范围内,R~2 0. 99,仪器检出限(IDL)为0. 040μg/L,方法检出限(MDL)为1. 60μg/kg。稻米和虾仁样品的加标回收率分别为84. 1%～98. 7%和89. 8%～109. 3%,相对标准差分别为2. 3%～10%和2. 2%～3. 1%。对产地不同的稻米和虾仁样品的实际检测显示,稻米无机硒含量分别为3. 88～45. 90μg/kg,占总硒的百分比最高值为11. 27%,虾仁样品无机硒含量为小于MDL～24. 76μg/kg,占总硒的百分比最高值为3. 83%。     

离子色谱-脉冲安培法测定芦荟多糖中7种单糖的含量

采用水提醇沉法提取芦荟鲜叶中的多糖，经三氟乙酸水解，利用Dionex CarboPac PA10高效阴离子色谱柱分离，氢氧化钠梯度淋洗，积分脉冲安培检测，建立了芦荟多糖中岩藻糖、鼠李糖、阿拉伯糖、半乳糖、葡萄糖、甘露糖和木糖7种常见单糖的测定方法。结果表明：7种单糖在线性范围内的相关系数（R²）均高于0.997，检出限为0.007~0.024 mg/L，加标回收率为97.5%~102.5%，相对标准偏差（RSD）为0.1%~4.8%。该法简单、快速、灵敏、准确，可用于芦荟多糖中单糖含量的测定和多糖组成的研究。     

Enterobacter Cloacae Z0206细菌胞外富硒多糖的抗氧化活性

利用产多糖菌Enterobacter cloacae Z0206(E.cloacaeZ0206)的深层发酵法制备了E.cloacae Z0206细菌富硒多糖;测定了其还原能力和清除1,1-diphenyl-2-picrylhydrazyl(DPPH)自由基、超氧阴离子及羟自由基的能力.结果表明,通过深层富硒发酵、醇沉离心等制备富硒多糖SEPS的产量为9.28g/L,富硒量为2.314mg/g;E.cloacae Z0206富硒多糖对DPPH自由基和羟自由基具有较好的清除作用,在浓度为5g/L时对DPPH自由基和羟自由基的清除率分别为80.35%和84.26%,并具有较强的还原能力,但其对超氧阴离子自由基的清除能力较差.     

柱前衍生高效液相色谱法分析新疆桃胶的多糖组成

采用超声波辅助提取,乙醇沉淀,三氯乙酸去蛋白的方法提取新疆8种桃胶中的多糖,将所得多糖用三氯乙酸进行水解并用1-苯基-3-甲基-5吡咯啉酮进行衍生化处理,采用反相高效液相色谱-紫外检测法研究桃胶多糖的单糖组成。结果表明,8种桃胶多糖主要由阿拉伯糖、半乳糖和木糖组成,还含有少量的葡萄糖醛酸、鼠李糖及甘露糖,不同品种的桃胶其多糖的单糖组成及含量存在一定差异。该方法简便,重现性良好,适合进行桃胶多糖的成分分析研究。     

梁王茶茎皮多糖提取工艺的优化及其抗氧化活性研究

本文为优化梁王茶茎皮多糖(PND)的提取工艺,并评价其抗氧化活性,以多糖提取率为评价指标,在单因素实验的基础上采用响应面法对超声时间、超声温度和超声功率三个影响梁王茶多糖提取工艺的主要因素进行优化;再通过DPPH、ABTS自由基清除实验和FRAP法评估其抗氧化能力。结果表明,超声提取梁王茶茎皮多糖的最佳工艺条件为超声时间120 min、超声温度60℃、超声功率125 W、浸泡时间20 min、液料比10∶1及乙醇浓度80%,该条件下多糖提取率为4.780%。抗氧化实验表明,梁王茶茎皮多糖浓度在1～10 mg·mL~(-1)范围内,随多糖浓度增加DPPH自由基清除能力增强,IC_(50)值为7.591±0.205 mg·mL~(-1);以Trolox当量来表示其ABTS自由基清除能力为1.464±0.194 mmol Trolox/g PND;以Fe~(2+)当量来表示其还原能力为0.302±0.020 mmol Fe~(2+)/g PND。     

UPLC-MRM法测定饲料中的三聚氰胺

提出了一种UPLC-MRM测定饲料中微量三聚氰胺的分析方法. 饲料经10 g/L三氯乙酸溶液提取和22 g/L乙酸铅溶液沉淀蛋白质, 过混合型阳离子交换柱(MCX)纯化, 离心后用0.45 μm滤膜过滤, 用超高效液相色谱-质谱-质谱联用仪(UPLC-MS-MS)分析测定, 以三聚氰胺母离子126.9 (m/z)和子离子67.5与84.6 (m/z)定性、定量目标物. 饲料样品加标回收率(n=6)为84.5%, 检测限0.01 μg/L, 相对偏差(RSD) 6.5%.     

动物源性食品中磺胺类药物增效剂残留的高效液相色谱-串联质谱法测定

利用高效液相色谱-电喷雾串联质谱测定了蜂蜜、蜂王浆、鮰鱼、鳗鱼、猪肉、猪肾、猪肝、鸡肉、牛肉和牛奶中的三甲氧苄氨嘧啶、二甲氧苄氨嘧啶和奥美普林3种磺胺类药物增效剂.除蜂王浆基质直接用10%三氯乙酸溶液提取外,其余基质均用10%三氯乙酸-乙腈(体积比7 : 3)混合溶液提取,提取溶液过阳离子交换固相萃取柱进行富集和净化.采用C18色谱柱,流动相为甲醇和0.1%甲酸溶液.选择1个母离子和2个子离子进行反应监测,对3种磺胺类药物增效剂残留进行定性,选择信号最强的子离子进行定量.在2 ～100 μg/L范围内,分析物的线性相关系数r>0.992.通过实际样品添加回收实验,所有基质定量下限为5.0 μg/kg,3个添加水平的回收率为63% ～89%,相对标准偏差为3.2% ～6.9%.     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

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.     

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.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.