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薯蓣属植物中薯蓣皂甙元的含量测定 总被引:5,自引:0,他引:5
以穿龙薯蓣(Dioscorea nipponica Makino)为对象,研究了根中薯蓣皂甙元的定量方法,并进一步試用于测定其他四种薯蓣植物。植物的根剪碎成小粒状,加酸迴流水解,用苯提取皂甙元,提出物經氧化鋁柱层离分出薯蓣皂甙元后,以改良Liebermann試剂显色,比色测定。本法簡便易行,結果稳定,适于作一般例行分析。 相似文献
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高三尖杉酯碱在大鼠及兔肝微粒体的代谢研究 总被引:1,自引:0,他引:1
采用动物肝微粒体体外代谢法对高三尖杉酯碱进行了代谢转化的研究。应用梯度洗脱—反相HPLC结合二极管陈列检测器对体外代谢体系进行了分析。判定在体外代谢体系中,高三尖杉酯碱主要产生一个代谢产物。用HPLC法制备出一定量代谢物纯品,经光谱分析及与化学制备的对照品相比较,推定其代谢物结构为:2′-羟基-2′(α-乙酸)-6′-甲基-6′-羟基-庚酰三尖杉碱。 相似文献
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洋地黄叶提出物在甲酰胺作固定相的硅藻土薄层上,用氯仿-丙酮-醋酸乙酯-乙醇-甲酰胺(8∶2∶0.5∶0.5∶饱和),或氯仿-丁醇-甲酰胺(9∶1∶饱和),或氯仿-醋酸乙酯-苯-甲酰胺(1∶3∶2∶饱和)作展开剂,分别分离毛花洋地黄一级甙,紫花洋地黄一级甙,或二级甙。展开后的板,于100℃烤去甲酰胺,碘蒸气显点,用吸取器将色点吸下,以呫吨氢醇的冰醋酸溶液洗脫。洗脫液中加入一定量盐酸后,显色测定。曾测定了六种纯强心甙的回收率,除羟基洋地黄毒甙因色点有拖尾,结果偏低,为87.7%外;毛花洋地黄甙甲、乙、丙,洋地黄毒甙,异羟基洋地黄毒甙等的回收率均在94.9—97.6%间,标准偏差0.6—2.6%。用本法测定了毛花洋地黄及紫花洋地黄二种干叶中的主要强心甙含量,结果与纸层离法基本一致,但本法操作时间可以大大缩短,误差小,而且也容易掌握。 相似文献
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A method for determining the total alkaloids of the Chinese drug Tsingjiu (秦艽) (Gentiana macrophylla) based on titration with silicotungstic acid was found. Weigh out accurately 2 g of pulverized (80 mesh) sample. Macerate it in a glass-stoppered flask with 50 ml of a mixture of chloroform-methanol-concentrated ammonia water (75: 25: 5) for 48 hours with occasional shaking. Take exactly 25 ml of the filtrate, evaporate and dissolve the residue in 0.6 N acetic acid, Impurities in the acetic acid solution are removed with lead acetate and the excess of Pb+2 is removed by sodium sulphate. The clear filtrate is adjusted to about 50 ml with an acidity at about 0.5 N. The solution is titrated with 0.01 M silicotungstic acid, using malachite green as an outside indicator. Results are calculated on gentianine (C10H9O2N). 相似文献
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王慕邹 《国外医学(药学分册)》1974,(6)
巴比妥、茶硷、甲基硫脲嘧啶等pK值为7~8,故为弱酸,各国药典所用的定量方法均比较繁琐。本文以二甲替甲酰胺作溶剂,丙醇钾作滴定剂进行非水滴定测定,方法简便,结果准确。二甲替甲酰胺具有较好的溶剂性能,介电常数较高,为惰性溶剂,而且所具极性对多数有机酸及其盐均有良好的溶解度。缺点是对水灵敏,在水存在下遇碱即水解。滴定剂也可用四丁基氢氧化铵溶液,但稳定性较差,而且价昂。 相似文献
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尿液中利尿剂、丙磺舒、咖啡因、匹莫林的固相提取和HPLC初筛分析 总被引:1,自引:0,他引:1
A solid-phase extraction and reversed phase high performance liquidchromatographic method(RP-HPLC) was developed for the rapid determination of 13 diuretics (bel-onging to five different pharmacological groups) ,probenecid, caffeine and pemoline in urine. Two mlurine sample was first adsorbed on a XAD-2 column, then eluted with ether--ethyl acetate(l: 1).The eluate was evaporated to dryness and reconstituted in methanol. The methanolic solution wasinjected into a HP LiChrosorb RP-18 column, using phosphate buffer (pH 3) and acetonitrile as the mo-bile phase and monitored at 216 nm, 230 nm, and 275 nm on a diode array ultraviolet detector. Theextraction recoveries of 16 drugs were above 75%. The limits of detection ranged from 0. 3~3.0μg/ml of urine. All drugs were separately administered to healthy volunteers, positive urine sampleswere collected, and urinary excretion--time curves of some drugs were reported. 相似文献
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本文报道了民间药大乌头及藤乌头类乌头的植物来源,前者属于乌头属乌头亚属乌头组中的显柱乌头系(Ser Stylosa)类植物,后者系同组的蔓乌头系(Ser Volubulia)类植物,药用部分为其块根。研究了生药中生物碱的高效液相色谱测定方法,用十八烷基键合相柱,以甲醇—水—三乙胺(75:25:0.2)作流动相,各生物碱均能基线分离。分析了属于这类乌头的十二种不同植物品种的生药块根,均含有滇乌碱类生物碱,从化学分类学上证明这两群乌头植物在亲缘关系上有较密切的联系。 相似文献
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