柴达木枸杞几种活性成分分析

通过紫外可见分光光度法分别测定了柴达木枸杞主要活性成分枸杞多糖和总黄酮的含量,并且采用反相高效逆流色谱法分析并计算了柴达木盆地枸杞中芦丁的含量,色谱条件:C18色谱柱(4.6 mm×250 mm,5 μm),以V(甲醇)∶V(0.4% H3PO4)=50∶50为流动相,流速:1.0 mL/min,柱温:30 ℃,检测波长:360 nm,采集时间20 min.测得柴达木枸杞中多糖、总黄酮、芦丁的含量分别为8.33%、1.05%、0.077%.     

青海枸杞子中微量元素含量的测定

测定了青海枸杞子中锌、铜、锰、铅、砷、铁、硒等微量元素的含量。结果表明,青海枸杞子中含锌18.65μg/g,铜15.62μg/g,锰6.24μg/g,铅1.03μg/g,砷0.24μg/g,铁19.68μg/g,硒2.15μg/g,人体必需微量元素含量丰富,是枸杞具有极为重要的保健、防病、治病功能的重要原因之一。     

枸杞润肤霜中两种酚酸类成分的高效液相色谱检测及质谱确证

建立了自制枸杞润肤霜中绿原酸和咖啡酸的高效液相色谱分析及液相色谱-串联质谱确证方法。枸杞润肤霜样品经甲醇超声提取,提取液离心处理后,取上清液经微孔滤膜过滤后测定。采用Aglient HC-C18色谱柱(250×4.6mm,5μm)分离,以甲醇-0.5%乙酸水溶液(27∶73,V/V)为流动相,等度洗脱,流速1.0mL/min,检测波长327nm。绿原酸、咖啡酸分别在3.3~250μg/mL、3~225μg/mL间线性关系良好(r=0.9993);平均加标回收率分别为98.28%、99.26%,相对标准偏差(RSD)均为1.93%。自制枸杞润肤霜中绿原酸、咖啡酸含量分别为0.0398 mg/g、0.0323mg/g。该方法快速、准确,适用于同时测定枸杞润肤霜中绿原酸、咖啡酸的含量。     

液相色谱-串联质谱法测定枸杞酒中11种PDE-5抑制剂和4种α-受体阻断剂

建立了基于超高效液相色谱-串联质谱法对枸杞酒中11种PDE-5抑制剂和4种α-受体阻断剂的快速筛查方法。样本经1%甲酸-甲醇提取,超声波水浴20 min助提,以Hypersil GOLD C18为分离柱,0.1%甲酸-水/甲醇为流动相,梯度洗脱,以超高效液相色谱-质谱联用仪在多反应监测模式（MRM）下分析。采用该方法,15种违禁药物可以在10 min分析完毕,各组分离子色谱图峰形良好,保留时间在2.21～7.76 min之间。各组分质量浓度在5～100μg/L线性范围内相关系数均大于0.99,检出限为32.5～60.6μg/kg,定量限为97.5～157.5μg/kg,在80、40、20μg/kg三个加标水平下15种违禁药物回收率为78.8%～118.8%,相对标准偏差均小于10%(n=6)。该方法具有操作简便、分析快速、基质干扰小等优点,适用于枸杞酒中多种壮阳类违禁药物的筛查。     

钙在体内是如何分布的

钙在人体中是无处不在的,其中99％钙以骨盐（羟磷灰石结晶）形式存在于骨骼和牙齿的釉质中,只有1％左右的钙分布于各种软组织和体液中。据测算,以体质量70kg的成年人为例,其骨骼钙含量为1300g,占钙总量的98．8％;牙齿含钙量约为7g,占钙总量的0．53％;细胞外液钙含量约1g,仅占体内总钙量的0．07％;软组织含钙量约7g,占钙总量的0．53％;血浆中钙含量为0．35g,占体内总钙量的0．02％。     

钙在体内是如何分布的

钙在人体中是无处不在的,其中99％钙以骨盐（羟磷灰石结晶）形式存在于骨骼和牙齿的釉质中,只有1％左右的钙分布于各种软组织和体液中。据测算,以体质量70kg的成年人为例,其骨骼钙含量为1300g,占钙总量的98．8％;牙齿含钙量约为7g,占钙总量的0．53％;细胞外液钙含量约1g,仅占体内总钙量的0．07％;软组织含钙量约7g,占钙总量的0．53％;血浆中钙含量为0．35g,占体内总钙量的0．02％。     

雄黄染毒后大鼠脑组织中氨基酸类神经递质含量的变化

研究了雄黄对大鼠脑组织氨基酸类神经递质含量的影响.将32只Wistar大鼠随机分为对照组(0.5%CMC-Na)以及低剂量(0.3g/kg)、中剂量(0.9g/kg)、高剂量(2.7g/kg)雄黄染毒组,通过连续灌胃给予雄黄混悬液两周.采用高效液相色谱-柱前衍生化法测定了大鼠脑组织中氨基酸类神经递质含量的变化.结果表明,与对照组比较,低剂量组大鼠脑组织中丝氨酸、甘氨酸和γ-氨基丁酸含量明显增加.中、高剂量组大鼠脑组织中同型半胱氨酸、谷氨酰胺、丝氨酸和天冬氨酸含量明显比对照组的低.总体而言,雄黄可对大鼠脑组织氨基酸类神经递质产生影响,氨基酸类神经递质可能是雄黄毒性作用的靶点之一.     

反相高效液相色谱法测定枸杞中类胡萝卜素及酯类化合物

建立了同时测定枸杞中类胡萝卜素及其酯类化合物含量的高效液相色谱分析方法,采用ODS-Cl8色谱柱(250 mm×4.6 mm;5 μm) ,流动相为甲醇-乙腈-二氯甲烷-正己烷(15402020,V/V)等度洗脱,二极管阵列检测器,检测波长为450 nm,流速1.0 mL/min,柱温25 ℃.外标法定量,玉米黄素、β-胡萝卜素、玉米黄素双棕榈酸酯3组分线性关系良好,相关系数0.9991～0.9998;平均回收率为98.8%～100.5%;RSD为0.8%～1.8%;检出限为0.02～0.20 mg/L.方法简便、快速、准确,可以用于枸杞类胡萝卜素定量测定.     

SPE-HPLC法测定枸杞中阿维菌素B1a残留量

建立了固相萃取前处理净化技术-高效液相色谱(HPLC)法检测枸杞中阿维菌素B1a残留量的方法.样品用乙腈提取,经C18固相萃取柱净化,采用C18柱(250 mm×4.6 mm i.d.,5 μm)分离,以V(甲醇):V(水)=85:15为流动相,在245 nm下进行检测.阿维菌素B1a在0.20～2.00 μg/mL范围呈良好的线性关系(γ=0.9994);该方法检出限(S/N=3)为0.02mg/kg;添加回收率为88.3%～102.5%,相对标准偏差为2.1%～3.8%.     

微波辅助萃取-GC/MS联用分析竹子中氨基酸

建立了微波辅助萃取-GC/MS联用测定竹子中谷氨酸、天冬氨酸和苯丙氨酸等10种氨基酸的分析方法, 优化了微波辅助萃取条件, 方法的线性范围在0.100～100 μg/mL之间, 检出限在0.0098～0.36 μg/mL之间, RSD为4.1%～9.7%, 回收率在84.3%～118%之间. 分析了4种不同产地、竹龄竹子的竹叶、竹枝和竹沥中氨基酸含量. 结果表明, 不同竹种、产地及竹龄的竹子中氨基酸总量有较大差异;相同竹种其竹沥中氨基酸含量显著高于竹叶及竹枝中氨基酸含量.     

Determination of Taurine in Lycium Barbarum L. and Other Foods by Capillary Electrophoresis with Electrochemical Detection

A method based on capillary electrophoresis (CE) with electrochemical detection (ED) was developed for the determination of taurine in Lycium Barbarum L., LIPOVIYAN beverage and milk powder. The effects of some important factors such as the acidity of the running buffer, separation voltage, injection time, and applied potential to working electrode were investigated. Operated in a wall‐jet configuration, a 300 μm diameter carbon‐disk electrode was used as the working electrode, which exhibits good responses at +1.05 V (vs. SCE) for taurine. Excellent linearity was obtained in the concentration range from 5.0×10^?4 mol/L to 5.0×10^?6 mol/L. The detection limit (S/N=3) was 1.0×10^?7 mol/L. This proposed method has been successfully applied to analyze the actual samples with satisfactory assay results.     

邻苯二甲醛-尿素柱前衍生高效液相色谱法快速检测枸杞中牛磺酸

干枸杞经粉碎、匀浆、离心后,通过阳离子交换柱脱去样品中其它氨基酸,再通过Ｚｏｒｂａｘ－Ｃ８柱进行柱前衍生分离。衍生剂：Ａ．４％ＯＰＡ甲醇溶液;Ｂ．尿素∶磷酸钠盐缓冲液（ｐＨ６．８）＝１∶３（Ｗ／Ｖ）。流动相：甲醇∶０．０１ｍｏｌ／Ｌ乙酸钠溶液（ｐＨ６．８）＝３５∶６５（Ｖ／Ｖ）。紫外检测波长３３０ｎｍ。牛磺酸浓度在０．１～１．０ｍｍｏｌ／Ｌ范围内可被定量测定。回收率可达１００．３１％±１．９８％,变异系数（ＣＶ）为１．９４％。     

大孔树脂分离纯化宁夏枸杞总黄酮的研究

考察了NKA-9、S-8、XDA-1、AB-8、HPD-100、HPD-600 6种大孔吸附树脂对宁夏枸杞总黄酮的吸附和解吸性能,筛选出XDA-1树脂的效果最佳;考察了pH值、样液浓度、流速等对XDA-1树脂静态吸附效果的影响;并进行了动态吸附试验,确定出XDA-1树脂动态吸附枸杞总黄酮的最佳条件:样品液浓度为0.25mg/mL,控制流速为0.5mL/min,样品液pH 5;最佳洗脱条件:洗脱液为80%的乙醇水溶液,用量为35mL (5倍柱床体积).在此条件下,枸杞总黄酮含量从27.2%提高到79.8%,回收率为87.4%,表明XDA-1树脂可用于宁夏枸杞总黄酮的分离纯化.     

Preparation of prunin with the help of immobilized naringinase pretreated with alkaline buffer

Immobilized naringinase can be converted to a preparation showing only rhamnosidase activity by treatment with 0.1M glycine-NaOH buffer, pH 12. A simple method is described to obtain pure prunin in high yield from naringin with the help of this immobilizate.     

One-pot preparation of Julia-Kocienski sulfides and sulfones from alcohols

A method for one-pot preparation of Julia-Kocienski sulfides and sulfones from alcohols and thiols is reported. A variety of primary alcohols were converted to the corresponding mesylates by methansulfonyl chloride and triethylamine in THF. After the reaction is complete, thiol (1 or 10) and either NaH or t-BuOK were added. The Julia-Kocienski sulfides 3, 9 and 11 were prepared by one-pot two steps procedure from alcohols in 76–96% yields (16 examples). Furthermore, after the sulfide formation, the reaction mixture was neutralized by p-toluenesulfonic acid and treated with H₂O₂ and ammonium molybdate in EtOH to give the Julia-Kocienski sulfones 4 in good yields except for trans-2-hexen-1-ol.     

Darstellung von Oxalatosilicaten aus SiO2

Preparation of Oxalatosilicates from SiO₂ Amorphous silica (aerosil, silica gel, or kieselguhr) reacts with oxalic acid under anhydrous conditions in presence of appropriate bases, forming oxalatosilicates. Tris(oxalota)silicates of triethylammonium, dicyclohexylammonium, triphenylphosphonium and K(18-crown-6) are obtained in high yields by this reaction.     

Multilayer effects in adsorption of alcohols from benzene andn-heptane on silica gel

Experimental data for the title systems are compared with calculations based on theoretical adsorption parameters.

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Mehrschichteffekte bei der Adsorption von Alkoholen aus Benzol undn-Heptan auf Silicagel (Kurze Mitteilung)

Zusammenfassung Für die im Titel genannten Systeme werden experimentelle Daten mit Berechnungen verglichen, die auf theoretischen Parametern basieren.

     

Recent progress in plant cell culture

Conclusions Commercial application of plant cell cultures for the production of useful metabolites on a large scale has not yet been realized. However, some recently published papers and patents seem very attractive for industrial use because their results and techniques are apparently applicable to a large-scale production of metabolites. The author believes that commercial success using plant tissue cultures will be realized in the near future with advanced techniques if product selection is determined by economic and political principles. In 1982, the 5th International Congress of Plant Tissue and Cell Culture will be held in Japan and this undoubtedly will encourage research activity in our country.     

Inelastic scattering of fast electrons from simple closed shell atoms. I. He,Be

The inelastic collision of fast electrons with ground state closed shell atoms is investigated within the context of First Born Approximation and Random Phase Approximation. Generalized oscillator strengths and total cross sections for 1¹ S n ¹ D transitions in He and 1¹ S n ¹ S in Be are evaluated and discussed.Work supported by Consiglio Nazionale delle Richerche (C.N.R.) through its Istituto di Chimica Quantistica ed Energetica Molecolare in Pisa.