快速制备液相色谱分离库拉索芦荟中10-羟基芦荟大黄素苷(英文)

采用快速制备液相色谱从库拉索芦荟中高效分离制备10-羟基芦荟大黄素苷A和B。以库拉索芦荟药材粉甲醇提取物为原料,采用快速制备液相色谱,EYELA柱(300 mm×20 mm i.d.,20~45μm),甲醇-水为流动相(35∶65,v/v)等度洗脱,流速10 mL/min,检测波长356 nm,对芦荟样品进行分离制备,得到2种化合物单体,经UV、旋光度、HRMS和NMR鉴定,HPLC测定纯度,2个化合物分别为10-羟基芦荟大黄素苷B(98.9%)和10-羟基芦荟大黄素苷A(98.2%)。该方法简便、快速,所得产物纯度较高,可用于对照品的制备和药理毒理活性研究。     

HPLC-DAD和LC-MS/MS法对各种芦荟样品中蒽醌类成分的分析研究

采用HPLC-DAD和LC-MS／MS对各种芦荟样品中蒽醌类成分进行鉴定,在此基础上建立了同时测定各种芦荟样品中芦荟苷与芦荟大黄素含量的方法。采用Nucleodur-silica色谱柱（250mm＊4．6mm,5μm）,流动相A为甲醇-醋酸（500：1．70）,B为水．醋酸（500：1．70）,梯度洗脱,流速1．0mL／min,DAD扫描波长范围为190～370nm,紫外检测波长为254和356nm。质谱离子源为ESI,采用全扫描一级质谱和选择离子全扫描二级质谱两种方式同时测定。结果表明：各种芦荟样品中主要的蒽醌类成分为芦荟苷A、B与芦荟大黄素,未检测到大黄素、大黄酸、大黄素甲醚、大黄酚;芦荟干粉中所含的芦荟苷含量最高。该法准确、可靠、重现性好,可行性高。     

中压液相色谱法快速制备木犀草素-7-O-β-D-葡萄糖醛酸苷单体及鉴别

本文采用二元中压制备液相色谱系统,以装有反相C18(Chromatorex,MB 100-40/75)分离填料的两端具有锥形不锈钢接口的耐压玻璃柱(φ49 mm×H310 mm)作为制备色谱柱,流动相为甲醇(A)/含0.05%冰醋酸水溶液(B),梯度洗脱程序:0~20 min,10%(A);20~230 min,30%(A);230~270 min,60%(A);270~300 min,100%(A),流速:50 mL/min,检测波长254 nm,进样量:200 mL,从抱茎苦荬菜(苦碟子)总黄酮中快速、高效地分离得到木犀草素-7-O-β-D-葡萄糖醛酸苷(L7GU)单体。所得单体经UV、IR、TOF-MS、1H NMR、13C NMR方法进行了结构确证。经硅胶和聚酰胺薄层色谱检查,在365 nm紫外灯下均呈单一的黄绿色荧光斑点;HPLC-UV分析表明,在210、254、290、348 nm四个波长下,采用色谱峰面积归一化方法计算产品纯度均在98%以上。所得产品可直接作为对照品用于苦碟子药材及制剂的质量控制。     

高速逆流色谱分离制备甘草中的甘草苷和芒柄花苷

应用高速逆流色谱分离制备甘草中的甘草苷和芒柄花苷。将甘草乙酸乙酯提取物经聚酰胺柱粗分后,30%乙醇洗脱物用高速逆流色谱进一步分离,所用两相溶剂系统为乙酸乙酯-水(5∶5,v/v),转速850 rpm,流速2.0 mL/min,检测波长254 nm,从50 mg30%乙醇洗脱物中得到甘草苷8.7 mg、芒柄花苷4.2 mg,纯度分别为99.5%和97.3%。所得产物的结构经核磁共振谱(NMR)鉴定。利用该方法可以对甘草中的甘草苷和芒柄花苷进行快速的分离和纯化。     

藏药短管兔耳草中松果菊苷和麦角甾苷的RP-HPLC分析

建立了藏药短管兔耳草中松果菊苷和麦角甾苷含量的高效液相色谱分析法.采用Waters XTerra RP18色谱柱(150mm×4.6 mm,5μm),以甲醇-1%冰醋酸溶液(28:72,V:V)为流动相,流速1.0 mL/min,检测波长330 nm,柱温30℃,在20 min内分离检测了该两种化合物.松果菊苷和麦角甾苷进样量分别在0.077～4.950μg(r=0.999 9)和0.085～5.450μg(r=0.999 9)内呈良好线性,平均加样回收率分别为98.35%和92.50%,RSD分别为2.35%和2.86%.所建立的方法简便、快捷、结果准确可靠,重现性好,可用于藏药短管兔耳草的质量控制,并为兔耳草属植物中苯丙素苷类化合物的分离分析提供一定的参考.     

中药库拉索芦荟化学成分的液质定性分析

为阐明中药库拉索芦荟(Aloe barbadensis)叶的汁液浓缩干燥物的化学成分,该研究采用HPLC-DAD-ESI-IT-TOF-MSⁿ技术,结合对照品对比和文献检索,对其进行系统的定性分析。以水(A)-乙腈(B)为流动相进行梯度洗脱,流速为1.0 mL·min^-1,质谱使用ESI离子源,采用负离子模式分析液质数据。结果表明：(1)首次阐明中药库拉索芦荟中蒽醌类(芦荟大黄素、大黄素甲醚、大黄素-8-O-β-D-吡喃葡萄糖苷)、蒽酮类(芦荟素A、芦荟糖苷A)、色酮类(芦荟新苷D、7-O-甲基芦荟新苷A、altechromone A、芦荟苦素、芦荟新苷G、芦荟新苷C)、α-吡喃酮类(芦荟宁A、芦荟宁B)四类成分的主要化合物的裂解途径。蒽醌类化合物的裂解途径以失去CO₂和CO为主,蒽酮类化合物的裂解途径以己糖苷的裂解和失去CO为主,色酮类化合物的裂解途径以己糖苷的裂解和酯基的水解为主,α-吡喃酮类的裂解途径主要包括己糖苷的裂解、CO₂和H₂O的丢失等。(2)共检测到168种化学...     

红树白骨壤果实中酚苷类化学成分研究

采用柱色谱、凝胶层析和高效液相色谱分离技术,从白骨壤果实中分离获得6个酚苷类单体化合物。运用波谱分析和文献对照方法,分别鉴定为Rhyncoside A(1)、松柏苷(2)、对羟基苯甲酰葡萄糖(3)、顺式香豆酸-4-O-β-D-吡喃葡萄糖苷(4)、香草酸4-O-β-D-吡喃葡萄糖苷(5)、苯基-β-D-葡萄糖苷(6)。化合物1-6均是首次从该种海洋植物中分离得到。     

毛脉酸模根中一新的色原酮苷类化合物

从毛脉酸模根(Rumex gmelini Turcz.)75%乙醇提取物中分离得到1个新色原酮苷和5个已知化合物,应用波谱学方法及文献对照分别鉴定为2,5-dimethyl-7-hydroxychromone-7-O-β-glucopyranoside (1),nepodin-8-O-β-D-glucopyranoside (2),10-hydroxyaloin A (3),10-hydroxyaloin B (4),5-methoxyl-1(3H)-benzofuranone-7-O-β-D-glucopyranoside (5),phenylethyl-O-α-L-arabinopyranosy-(1→6)-O-β-D-glucopyranoside (6). 其中化合物1为新化合物,3～6首次从酸模属中分离得到,化合物2首次从该植物中分离得到.     

刺五加叶中金丝桃苷含量的测定

用高效液相色谱法测定了刺五加(Acanthopanax senticosus(Rupr.&Maxin)Harms)叶中金丝桃苷(hyperin)的含量。色谱柱为C18柱,流动相为甲醇和0.025mol L-1磷酸,比例为V甲醇:V0.025mol.L-1磷酸.=55:45(混合后用三乙胺调pH3.0￣3.2),检测波长360nm。样品用甲醇超声提取。结果表明,金丝桃苷峰形良好,与其他组分的色谱峰达到基线分离。加样回收率为104%,相对标准偏差RSD为5.38%。本研究为刺五加叶中金丝桃苷含量的测定建立了一种可靠的方法。     

刺五加叶中金丝桃苷含量的测定

用高效液相色谱法测定了刺五加(Acanthopanax senticosus (Rupr.& Maxin) Harms)叶中金丝桃苷(hyperin)的含量。色谱柱为C18柱,流动相为甲醇和0.025 mol.L-1磷酸,比例为V甲醇:V0.025 mol.L-1磷酸=55:45 (混合后用三乙胺调pH3.0～3.2),检测波长360 nm。样品用甲醇超声提取。结果表明, 金丝桃苷峰形良好,与其他组分的色谱峰达到基线分离。加样回收率为104%,相对标准偏差RSD为5.38%。本研究为刺五加叶中金丝桃苷含量的测定建立了一种可靠的方法。     

Inhibition of collagenase and metalloproteinases by aloins and aloe gel

The effects of Aloe barbadensis gel and aloe gel constituents on the activity of microbial and human metalloproteinases have been investigated. Clostridium histolyticum collagenase (ChC) results dose-dependently inhibited by aloe gel and the activity-guided fractionation led to an active fraction enriched in phenolics and aloins. Aloins have been shown to be able to bind and to inhibit ChC reversibly and non-competitively. Aloe gel and aloins are also effective inhibitors of stimulated granulocyte matrix metalloproteinases (MMPs). The remarkable structural resemblances between aloins and the pharmacophore structure of inhibitory tetracyclines, suggest that the inhibitory effects of aloins are via an interaction between the carbonyl group at C(9) and an adjacent hydroxyl group of anthrone (C(1) or C(8)) at the secondary binding site of enzyme, destabilizing the structure of granulocyte MMPs.     

Synthesis of gold nanotriangles and silver nanoparticles using Aloe vera plant extract

Biogenic gold nanotriangles and spherical silver nanoparticles were synthesized by a simple procedure using Aloe vera leaf extract as the reducing agent. This procedure offers control over the size of the gold nanotriangle and thereby a handle to tune their optical properties, particularly the position of the longitudinal surface plasmon resonance. The kinetics of gold nanotriangle formation was followed by UV-vis-NIR absorption spectroscopy and transmission electron microscopy (TEM). The effect of reducing agent concentration in the reaction mixture on the yield and size of the gold nanotriangles was studied using transmission electron microscopy. Monitoring the formation of gold nanotriangles as a function of time using TEM reveals that multiply twinned particles (MTPs) play an important role in the formation of gold nanotriangles. It is observed that the slow rate of the reaction along with the shape directing effect of the constituents of the extract are responsible for the formation of single crystalline gold nanotriangles. Reduction of silver ions by Aloe vera extract however, led to the formation of spherical silver nanoparticles of 15.2 nm +/- 4.2 nm size.     

Isolation and characterization of novel protein with anti-fungal and anti-inflammatory properties from Aloe vera leaf gel

The Aloe protein of 14 kDa from the Aloe vera leaf gel was isolated by an ion exchange chromatography using DEAE-cellulose and CM-cellulose column. The purified Aloe protein exhibited a potent anti-fungal activity against Candida paraprilosis, Candida krusei and Candida albicans. In addition, the purified Aloe protein also showed an anti-inflammatory property against pure lipoxygenase and cyclooxygenase-2 with 84% and 73% inhibition, respectively, and was verified by binding with these proteins by real time method by the phenomenon of surface plasmon resonance. This Aloe protein is a novel protein possessing antifungal and anti-inflammatory properties and thus sets a platform to be used as a medicinal plant product.     

库拉索芦荟幼苗对海水胁迫的响应

采用砂培试验,研究库拉索芦荟（Aloe vera）幼苗对海水胁迫的响应特征。结果表明：（1）30％海水处理20d,库拉索芦荟幼苗的干重与对照无显著差异,而30％海水处理库拉索芦荟的根干重明显高于10％海水及淡水处理;（2）海水胁迫下,库拉索芦荟幼苗中离子区域化明显：从地下部和地上部来看,Na^＋、Cl^＋明显在芦荟根部积累,海水比例越高,根部Na^＋、Cl^＋含量越大,而K^＋却相反;海水胁迫下芦荟地上部分功能叶片中Na^＋、Cl^＋含量最低,K^＋含量最高,而淡水处理从老叶到新叶,Na^＋、Cl^＋含量总是呈下降趋势,而K^＋正好相反;随海水胁迫在库拉索幼苗中Ca^2＋含量下降,而Mg^2＋含量七升;（3）随海水胁迫时间增加芦荟叶片质膜透性呈显著上升,MDA含量呈波动变化。     

Separation and determination of astaxanthin from microalgal and yeast samples by molecularly imprinted microspheres

In this work, molecularly imprinted microspheres (MIMs) were synthesized by aqueous microsuspension polymerization using astaxanthin (3,3'-dihydroxy-beta,beta'-carotene-4,4'-dione) as imprinting molecule. The MIMs obtained were subsequently packed into the stainless steel column and the chromatographic characterization of the column was investigated. The effects of pH and composition of the mobile phase on the retention factor (k') were investigated in detail. The mixture of methanol and dichloromethane (DCM) (8:2, v/v) was used as mobile phase A while the mixture of methanol and water (5:5, v/v) as mobile phase B. The separation of astaxanthin and zeaxanthin (3,3'-dihydroxyl-beta-carotene) was obtained when the concentration of mobile phase B was higher than 30% (v/v) due to their strong lipophilicity. The method developed was successfully applied to separate astaxanthin in the saponified samples of the microalga Haematococcus pluvialis and the yeast Phaffia rhodozyma. The recovery of adding 40 mg astaxanthin to 1.0 g microalgal sample was 95.5% with an R.S.D. (n =5) of 5.3%. The results of determination of astaxanthin in the microalga and the yeast were 3.7% (R.S.D (n = 1.5%, n = 9) and 0.041% (R.S.D n= 7.3%, n = 9), respectively.     

芦荟维管束的结构与芦荟素积累的相关性

应用半薄切片、组织化学、荧光显微镜观察和薄层层析 (TLC)相结合的方法研究了中华芦荟 (Aloeve-ra L.var.chinensis)、木立芦荟 (Aloe arborescens)叶和茎内维管束的结构及其与芦荟素积累的关系。结果表明 ,木立芦荟叶内维管束和中华芦荟叶内外轮的维管束中有大型韧皮薄壁细胞 ,而木立芦荟茎和中华芦荟叶中内轮维管束无大型韧皮薄壁细胞。组织化学结果表明 ,用醋酸铅处理过的上述材料 ,大型韧皮薄壁细胞内出现沉淀物 ;在荧光显微镜下经蓝光激发 ,大型韧皮薄壁细胞发出桔黄色荧光 ,都显示出芦荟素反应。薄层层析(TLC)结果证明 ,木立芦荟和中华芦荟叶含有大型韧皮薄壁细胞的维管束都含芦荟素 ,而木立芦荟茎及中华芦荟叶中内轮维管束都不含芦荟素。为此 ,维管束中的大型韧皮薄壁细胞与芦荟素的积累密切相关 ,维管束中是否有大型韧皮薄壁细胞可作为判断是否含有芦荟素的解剖学指标。     

Simultaneous determination of olanzapine,clozapine and demethylated metabolites in serum by on-line column-switching high-performance liquid chromatography

An automated method for simultaneous routine quantification of the antipsychotic drugs clozapine, olanzapine and their demethylated metabolites is described. The method included adsorption on a cyanopropyl (CPS) coated clean-up column (10 μm; 10×2.0 mm I.D.), washing off interfering serum constituents to waste, and separation on C18 ODS Hypersil reversed phase material (5 μm; 250×4.6 mm I.D.) using acetonitrile–water–tetramethylethylenediamine (37:62.6:0.4, v/v/v) adjusted to pH 6.5 with concentrated acetic acid. UV-detection was performed at 254 nm. The limit of quantification was 10–20 ng/ml. Relative day to day standard variations ranged between 4.5 and 13.5%. The method is suitable for routine monitoring of olanzapine and clozapine including their demethylated metabolites.     

芦荟属植物种间杂交及其F_1代POD同工酶鉴定

以芦荟属植物元江芦荟和皂质芦荟为亲本进行远缘有性杂交试验。正交对3株103朵小花进行授粉,获得7枚果实,平均结实率为6.80%;反交对2株88朵小花授粉,获得5枚果实,平均结实率为5.88%。获得了19株F1代实生苗,并对亲本和F1代实生苗以及库拉索芦荟、华芦荟等5种芦荟属植物进行了过氧化物酶同工酶(POD)的比较研究,结果显示,5种芦荟种间的POD同工酶酶谱具有较高的相似程度,同时各种又具有各自的特征酶带,很容易区分。特别是F1代实生苗的酶谱与父母本的酶谱有显著不同的酶带,证明产生了新的中间类型。     

芦荟凝集素的分离、纯化和部分性质的研究

新鲜芦荟叶（Ａｌｏｅ ｖｅｒａ Ｌ．ｖａｒ．ｃｈｉｎｅｎｓｉｓ（Ｈａｗ．）Ｂｅｒｇｅｒ）于室温用低浓度ＮａＣｌ溶液提取。离心和透析后,经Ｎ－乙酰氨基葡萄糖０Ｓｅｐｈａｒｏｓｅ ４Ｂ亲和层析,分离纯化出芦荟凝集素（ＡＣＬ）。用ＳｅｐｈａｄｅｘＧ－１００测表观分子量为３５ＫＤ,ＳＤＳ－ＰＡＧＥ出现两条色带;染色 ;宽带和较浅的罕带。亚基分子量分别为１５ＫＤ和２０ＫＤ。能专一性凝集兔血细胞和人血红细胞     

Assessment of chronic administration of aloe vera gel on haematology, plasma biochemistry, lipid profiles and erythrocyte osmotic resistance in wistar rats

The study was designed to investigate the effects of chronic administration of Aloe vera gel extract on markers of hepatic damage, lipid profiles and erythrocyte osmotic fragility using the Wistar rats. Forty male Wistar rats divided into four groups of ten rats per group were used in the study. Group I which served as the control received 0.9% physiological saline while those in groups II, III and IV received Aloe vera gel (100, 250 and 500mg/kg), respectively, for four weeks. There was significant increase in the haemoglobin concentration while the PCV, RBC count, MCH and MCHC though showed some marginal increases but the increases were not significant in all the treated rats. No significant change was also observed in the erythrocyte osmotic fragility. However, there were significant reductions in plasma ALT, AST and ALP levels in animals that received the gel compared with the control while the plasma albumin and total protein values were higher than those of the control. All the animals that received the gel also showed significant reduction in plasma total cholesterol, triglycerides and LDL-cholesterol ratio compared with the control. In a similar manner, those animals that were administered with 500mg/kg gel had significantly higher HDL-cholesterol ratio than those of the control. This study showed that, chronic administration of Aloe vera gel extract had no significant effects on the haematological parameters of the rats and did not affect erythrocyte osmotic resistance. It however showed some cholesterol lowering action.keywords: Aloe vera, Haematology, Osmotic fragility, Plasma biochemistry.