紫杉醇提取纯化工艺

以云南红豆杉树皮（或树叶）为原料，提取纯化紫杉醇。先经９５％乙醇、二氯甲烷提取，再经硅藻土柱涂渍色谱、硅胶６０中压快速柱色谱分离，收集含紫杉醇－ｃｅｐｈａｌｏｍａｎｎｉｎｅ的组分后以Ｃ_（１８）制备型ＲＰ－ＨＰＬＣ分离，两次结晶后得到紫杉醇无色结晶固体，纯度≥９８．８％，收率为树皮干重的０．０２８％，树叶干重的０．００８８％。     

HPLC法同时测定人血浆中地尔硫卓及其代谢产物

本法用ＷａｔｅｒｓＢａｓｅｌｉｎｅ８１０色谱工作站，Ｗａｔｅｒｓ径向加压柱（Ｎｏｖａ－ＰａｋＣ＿（１８）８ｍｍ×１０ｃｍ，４μｍ），检测波长ＵＶ２３８ｎｍ，流动相为甲醇－水－二氯甲烷－０．１ｍｏｌ／Ｌ醋酸铵（６４：２３．５：２．５：１０），流速：２．０ｍｌ／ｍｉｎ；血样用混合溶剂一次提取，地尔硫和去乙酰地尔硫的提取回收率分别为８５．２％、８２．３％，平均方法回收率分别为９９．６％、１０１．１％，最低检测浓度均为５ｎｇ／ｍｌ。     

反相高效液相色谱法测定血浆中左旋四氢巴马汀浓度

本文建立了测定血浆中左旋四氢巴马汀浓度的反相高效液相色谱法。采用国产ＹＷＧ－Ｃ１８填充柱，以甲醇－水（７０：３０）为流动相，安定作内标，在紫外检测器２８１ｎｍ波长处进行监测，按内标法定量。血样用二氯甲烷提取。最低检测浓度为０．０６μｇ／ｍｌ，线性范围０．６２５～４０μｇ／ｍｌ，日内日间测定的ＲＳＤ小于６．９％。     

石蒜科生物碱的研究Ⅻ.薄层色谱鉴别石蒜生物碱和高效液相色？…

目的：研究健谈鉴别石蒜科生物碱加兰他敏和力可拉敏（二氢加兰他敏）及加兰他敏含量测定的方法。方法：采用硅胶薄层色谱分离鉴别石蒜生物碱，以二氯甲烷－甲醇－氨水（９０：１０：０．５）展开，稀碘化铋钾调剂显色；高效液相色谱汉采用硅胶柱，流动相为二氯甲烷－甲醇（１００：８），检测波长为２５４ｎｍ，线性范围为８０￣３２０μｇ，ｒ＝０．９９９６。结果：硅胶薄层色谱可分离临别石蒜生物碱加 他敏和力可拉敏，硅胶柱高     

高效液相色谱法测定4－［4″－（2″，2″，6″，6″－四甲基哌啶氮氧自由基）氨基］－4＇－去甲表鬼臼毒素大鼠血浆浓度及药代动力学参数

建立了大鼠血浆中４－［４″－（２″，２″，６″，６″－四甲基哌啶氮氧自由基）氨基］－４＇－去甲表鬼臼毒素（ＧＰ－７）浓度的ＨＰＬＣ测定方法。用ＯＤＳ柱分离，甲醇－水－冰醋酸（５９：４１：０．６）为流动相，检测波长２８５ｎｍ。血浆甲乙醚－二氯甲烷混合液萃取，４５℃水浴蒸干，残渣用流动相溶解进样，内标法定量；血药浓度在２～２００μｇ·ｍｌ－１范围内呈线性关系，ｒ＝０．９９９７，血浆最低检测浓度０．２μｇ·ｍｌ－１，方法回收率９４％～１００％，日内、日间ＲＳＤ２．２９％～７．７０％。大鼠ｉｖＧＰ－７１０，２０，３０ｍｇ·ｋｇ－１，药代动力学过程符合二室开放模型，消除半衰期为３９．８±１０．８ｍｉｎ。     

HPLC法测定人血浆及尿中溴莫普林浓度

反相ＨＰＬＣ法测定人血浆及尿中溴莫 浓度。血浆及尿样经二氯甲烷取等预处理后,于ＳｙｍｍｅｔｒｙＣ１８柱上,以甲醇－０．０２ｍｏｌ／ＬＮＨ４Ｈ２ＰＯ４（６０：４０,ｐＨ７．６０）为流动相进行分离测定。线性范围０．０５－４ｍｇ／Ｌ萃取回收率８２．４％－８６．１％加样回收率９６．６％－１００．９％,日内ＲＳＤ１．７２％－３．８１％,日间ＲＳＤ３．１０％－７．６３％。。本法准确可靠,适于在溴莫普林药动学等     

HPLC同时测定莲子心中莲心碱和甲基莲心碱的含量

用ＨＰＬＣ法同时测定了莲子心中莲心碱和甲基莲心碱的含量。色谱系统流动相为二氯甲烷－异丙醇－二乙胺（７５∶２５∶０．２），紫外检测波长２８２ｎｍ，方法的平均回收率分别为９９．６％和１０１．２％，ＲＳＤ分别为０．８０、１．５８％。     

比格犬血浆中托烷司琼的HPLC法测定

建立了比格犬血浆样品中托烷司琼的反相高效液相色谱检测法。血浆样品，加入盐酸三环哌酯作内杯，用乙酸乙酯提取，经稀盐酸反洗，再用二氯甲烷提取。色谱条件：Ｃ８柱；流动相：甲醇－水（５５：４５），加０。３％三乙胺，用冰醋酸调ｐＨ７．２，检测波长２８３ｎｍ。线性范围５．４５￣７００ｎｇ／ｍＬ，最低检测浓度为３．０ｎｇ／ｍＬ，回收率为７９．９％￣８５．８％，日内ＲＳＤ为１．０６％￣４．２７％，日间ＲＳＤ为２．     

HPLC法测定马钱子及其制剂中士的宁与马钱子碱的含量

报道了采用ＨＰＬＣ法测定马钱子及其制剂中士的宁与马钱子碱的含量。色谱填料为硅胶，流动相为正己烷－二氯甲烷－甲醇－浓氨试液（４７．５：４７．５：０．３５），检测波长为２５４ｎｍ。实验结果表明，该方法简便，准确，灵敏度高，重现性好。     

氨苄青霉素钠中有机溶媒残留量的测定与考察

本文用气相色谱法考察测定了全国７个生产厂家２２个批号的氨苄青霉素钠有机溶媒残留量，色谱条件为１０％的聚乙二醇（ＰＥＧ）－１００００和３．５％－缩二甘油（ＤＧ）混合玻璃色谱柱，柱温６５℃，ＦＩＤ检测器，以正内醇为内标，测定结果，残留溶媒及残留量主要有异丙醇０．０１９％～０．４１０％，二氯甲烷０．０２５％～０．０５１％，丙酮０．００３％～０．００６％。     

红豆杉中紫杉醇的高效液相色谱法测定(英文)

本文研究了高效液相色谱法测定红豆杉Taxus chinensis中紫杉醇的含量,以倍他米松作内标,在填充以YWG 80(10μm)固定相的不锈钢色谱柱上,以CH₂Cl₂-MeOH(95:5)作流动相,在UV 228 nm波长进行检测,其变异系数小于2%。     

Identification of a novel cardenolide (2''-oxovoruscharin) from Calotropis procera and the hemisynthesis of novel derivatives displaying potent in vitro antitumor activities and high in vivo tolerance: structure-activity relationship analyses

Analysis of the methanolic extract of Calotropis procera root barks enabled the identification of a novel cardenolide (2'-oxovoruscharin) to be made. Of the 27 compounds that we hemisynthesized, one (23) exhibited a very interesting profile with respect to its hemisynthetic chemical yield, its in vitro antitumor activity, its in vitro inhibitory influence on the Na+/K+-ATPase activity, and its in vivo tolerance. Compound 23 displayed in vitro antitumor activity on a panel of 57 human cancer cell lines similar to taxol, and higher than SN-38 (the active metabolite of irinotecan), two of the most potent drugs used in hospitals to combat cancer.     

Distribution and amounts of taxol in different shoot parts of Taxus cuspidata.

Different fresh shoot parts of male and female plants of Taxus cuspidata were extracted and analysed for taxol concentration by high performance liquid chromatography (HPLC). Extracted parts included: young needles (first 10 top needle pairs of 30 cm long branches), old needles (last 10 needle pairs of 30 cm long branches), green bark, dark bark (with intense secondary growth), young wood (originally surrounded by green bark), wood (originally surrounded by dark bark), young stems (surrounded by green bark and devoid of needles), and mature male cones. Dichloromethane extracts were analysed by HPLC and diode array spectroscopy. Taxol identification was done by retention time, U.V. spectra, and spiking with an authentic taxol standard; 1H-NMR analysis was done for needle extracts. All parts except male cones had measurable amounts of taxol; no effect of plant sex on taxol levels of the plant parts analysed was observed. Results indicated that the bark accounted for almost all the taxol present in stems devoid of needles. Needles showed the highest levels of taxol (overall average of 0.035 +/- 0.006% of the extracted dry weight), significantly higher than those displayed by dark bark samples (0.012 +/- 0.001% of the extracted dry weight). Different needle post-harvesting procedures were evaluated in relation to taxol yields, 96 h dark incubation at -12 degrees C and 96 h dark incubation at 25 degrees C under vacuum gave taxol yields equivalent to those of freshly extracted samples. However, results obtained for 96 h dark incubation at 60 degrees C indicated some extent of taxol degradation.     

Metabolism of inhaled dihalomethanes in vivo: differentiation of kinetic constants for two independent pathways

Dihalomethanes are metabolized by two major pathways: an oxidative, cytochrome P-450-mediated pathway that has been previously thought to yield only CO, and a glutathione (GSH)-dependent one that yields CO2. Both give 2 mol of halide ion. We studied the kinetic properties of the two pathways in vivo by exposing male rats to various inhaled concentrations of CH2Cl2,CH2F2, CH2FCl, CH2BrCl, and CH2Br2 and determining end-exposure carboxyhemoglobin (HbCO) and plasma bromide (where appropriate). Closed atmosphere gas uptake studies were employed for CH2F2, CH2FCl, CH2Cl2, and CH2BrCl metabolism. A physiologically based kinetic model was used to determine kinetic constants based on gas uptake or plasma bromide data and these constants were used to predict HbCO concentrations. Oxidation was high affinity, low capacity. The maximum metabolic rates for this pathway with CH2Br2, CH2BrCl, and CH2Cl2 were, respectively, 72, 54, and 47 mumol metabolized/kg/hr. CH2FCl did not undergo significant oxidative metabolism and appears more like CH3C1 than a dihalomethane in its metabolic reactivity. The GSH pathway was low affinity, but high capacity and could be described as a single first-order process at all accessible exposure concentrations. The rate constant for this first-order GSH-dependent pathway was related as CH2BrCl greater than CH2Cl2 congruent to CH2FCl greater than CH2Br2 greater than CH2F2. Presumably bromide is a preferred leaving group but steric hindrance in the initial reaction with GSH is important with CH2Br2. We also studied the effects of pyrazole (which inhibits microsomal oxidation) and 2,3-epoxypropanol (which depletes GSH) on dihalomethane metabolism. Pyrazole abolished CO production from CH2Br2, CH2BrCl, and CH2Cl2. GSH depletion did not change the yield of halide ion from the high-affinity pathway; it did increase the steady-state HbCO concentrations with CH2Cl2 and CH2ClBr, but not with CH2Br2. The putative formyl chloride (FC) intermediate from CH2Cl2 or CH2BrCl appears to have a longer life than the formyl bromide from CH2Br2 and a significant portion of the FC (congruent to 20-30%) may react with other cellular nucleophiles instead of spontaneously decomposing to CO. This portion of the oxidative pathway probably yields CO2.     

榅桲果实及种子不同提取部位的蛋白酪氨酸磷酸酶1B抑制活性筛选

目的探讨榅桲果实和种子的甲醇提取物及其不同溶剂提取部位对蛋白酪氨酸磷酸酶1B(PTP1B)的抑制作用,筛选抗糖尿病活性部位。方法利用PTP1B体外筛选系统,对榅桲果实和种子不同提取部位进行细致筛选,确定其降糖活性部位。结果榅桲果实和种子各部位均有不同程度抑制PTP1B活性的作用,其中榅桲种子乙酸乙酯部位、榅桲果实二氯甲烷部位和榅桲果实水部位的体积分数为50%的乙醇溶液洗脱部位对PTP1B抑制作用强,其半数抑制质量浓度(IC50)分别为0.844,0.423和0.395mg·L-1,初步推测榅桲果实及种子提取物具有抗2型糖尿病的潜力。结论榅桲种子乙酸乙酯部位、榅桲果实二氯甲烷部位和榅桲果实水部位的体积分数为50%的乙醇溶液洗脱部位是主要的抗糖尿病活性部位。     

Phenolic compounds with anti-inflammatory activity from Eupatorium buniifolium.

Anti-inflammatory activity was detected in the CH(2)Cl(2) extract of the aerial parts of Eupatorium buniifolium using the TPA-mouse ear model. Three compounds isolated from this extract, by bioassay-guided fractionation, significantly inhibited the inflammatory response. The compounds were identified as 5,7,5'-trihydroxy-3,6,2',4'-tetramethoxyflavone (1), scopoletin (2) and centaureidin (3) which inhibited the edema by 67.3 %, 59.8 % and 49.7 %, respectively, at a dose of 1 mg/ear.     

Growth Inhibition of Asexual Erythrocytic Forms of Plasmodium falciparum and P. berghei in vitro by Naphthylisoquinoline Alkaloid-Containing Extracts of Ancistrocladus and Triphyophyllum Species

Naphthylisoquinoline alkaloid-containing extracts [1–20] of four species of the genus Ancistrocladus (A. barteri, A. heyneanus, A. robertsoniorum, and A. tectorius) and of Triphyophyllum peltatum have been examined for their antiplasmodial activity against asexual erythrocytic forms of Plasmodium falciparum (NF 54, clone A1A9) and P. berghei (Anka) in vitro. Incorporation of 3 H-hypoxanthine was measured in the presence of the test substances. The above mentioned plant species are used in several countries of the pantropical area against fevers and malaria. Five of the examined extracts displayed high growth inhibiting activity in the P. falciparum system : CH 2 Cl 2 /NH 3 bark extract of T. peltatum [20], EtOH leaf extract of A. barteri [4], CH 2 Cl 2 leaf [14] and CH 2 Cl 2 /NH 3 bark [15] extracts of A. tectorius, and CH 2 Cl 2 leaf [17] extract of T. peltatum). These extracts (IC 50 < 1 µg/ml) [4, 14, 15, 17, and 20] were further examined in the P. berghei system. Two of them (the CH 2 Cl 2 /NH 3 bark extracts of A. tectorius [15] and T. peltatum [20]) were proven to be highly active in both test systems. These findings confirm that extracts of species belonging to the Ancistrocladaceae and the Dioncophyllaceae have a considerable antiplasmodial capacity.     

栽培曼地亚红豆杉针叶化学成分的分离与鉴定

目的对栽培于辽宁本溪的曼地亚红豆杉(Taxus media‘Hicksii’)针叶的化学成分进行研究。方法曼地亚红豆杉针叶的乙醇提取物经大孔树脂、硅胶柱色谱、ODS柱色谱、凝胶柱色谱进行分离纯化,依据1H-NMR、13C-NMR、ESI-MS、HRESI-MS鉴定其结构。结果从曼地亚红豆杉针叶的乙醇提取物中分离纯化得到6个化合物,分别鉴定为二萜类化合物:5-cinnamoyl-9-acetyltaxicin-I(1)、5-cinnamoyl-10-acetyltaxicin-I(2)、5-去桂皮酰基紫杉宁J(3)、紫杉醇(4);黄酮类化合物:柚皮素(5);脂肪酸类:十六烷酸(6)。结论化合物1、2、5和6为首次从曼地亚红豆杉中分离得到。     

红豆杉浸膏在氧化铝催化下紫杉醇的生成研究

目的 :研究在氧化铝层析初分离红豆杉浸膏中紫杉醇增量的来源。方法 :采用C18 硅胶反相层析、氧化铝层析及硅胶层析等方法对物料进行处理 ,HPLC分析紫杉醇的含量。结果 :紫杉醇增量主要来源于红豆杉浸膏中 7 表 紫杉醇的碱性氧化铝催化下的异构化。结论 :优化 7 表 紫杉醇的异构化条件 ,可以增加 7 表 紫杉醇向紫杉醇的转化。     

10-去乙酰基-7-表紫杉醇转化为紫杉醇的研究

目的将天然紫杉烷类物质10-去乙酰基-7-表紫杉醇高效地转化为抗癌药物紫杉醇.方法首先将10-去乙酰基-7-表紫杉醇中的2'-OH选择性保护、7-OH乙酰化、去保护3步一锅反应获得7-表紫杉醇,再在DBU的催化下差向异构化为紫杉醇.结果本方法以10-去乙酰基-7-表紫杉醇为起始原料,以40%的总收率制备得到紫杉醇.结论建立了一条将天然紫杉烷类物质以较高的化学选择性以及良好的收率转化为紫杉醇的途径.