高三尖杉酯碱在大鼠及兔肝微粒体的代谢研究

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。     

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

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.     

弱酸在非水介质中的滴定

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。     

三尖杉酯碱类的高速液相色谱法分离与测定

本文报道以Lichrosorb SI-60及Nucleosil C-18为固定相,用正相和反相高速液相色谱法分离三尖杉总生物碱、混合酯碱、及半合成三尖杉酯碱差向异构化合物,并用于混合酯碱、半合成三尖杉酯碱差向异构化合物的含量测定,比较了各种参数变化对色谱过程的影响,以拟定的方法对各种酯碱提取物、制剂及半合成产品作了定量分析。本法的灵敏度为1×10^-6g,平均偏差1.9%。     

洋地黄叶的分析——Ⅱ.薄层层离测定

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。     

中药秦艽中总生物碱的含量测定

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).     

薯蓣属植物中薯蓣皂甙元的含量测定

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。     

棉酚的高效液相色谱测定

本文介绍在离子交换键合相柱上,以柠檬酸盐缓冲液—甲醇系统分离测定棉酚中一些难于用其它系统分离的微量杂质的高效液相色谱法,并用此方法测定了棉花植物及各种棉酚样品中棉酚的含量。     

高效液相色谱法测定桂枝中3种有效成分的含量

目的:建立HPLC法测定桂枝中桂皮醛、栓皮酸和邻甲氧基栓皮醛的含量。方法:采用ODS色谱柱(150mm×4.6mm,5μm),以甲醇-水-冰乙酸(45:55:0.05)为流动相,流速为0.8 mL·min~(-1),紫外检测波长为280 nm。结果:栓皮醛、桂皮酸和邻甲氧基桂皮醛的线性范围(n=5)分别为0.125～2μg(r=0.999 8),0.003 2～2 μg(r=0.999 9),0.012 5～0.2μg(r=0.999 7),平均回收率(n=9)分别为99.3％,102.8％,98.9％。提取方法为甲醇冷浸12h。结论:本方法简便、准确,可为评价不同产地的桂枝质量提供依据。