大鼠脑组织单胺类递质及其代谢产物的检测方法研究

目的 :研究大鼠脑组织中单胺类递质及其代谢产物的高效液相反相离子对色谱测定法。方法 :采用LiChrosorbC18,10 μm色谱柱 ,流动相为甲醇 :水 (4 0 :60 ) ,含 0 .0 2 8g LEDTANa2 ,0 .15g LSDS ,0 .2ml LH2 SO4(pH 2 .5～ 3 ) ,荧光检测波长 :λEX=2 85 ,λEM=3 3 3。结果 :对 87只大鼠脑组织中 4种单胺类递质及其代谢产物的含量进行了同时测定 ,高香草酸 (HVA) 2 .5 0～ 40 .0 μg ml、去甲肾上腺素 (NE) 0 .0 1～ 0 .5 0 μg ml、多巴胺 (DA)0 .0 5～ 1.0 0 μg ml、5 羟色胺 (5 HT) 0 .0 2 5～ 0 .5 0 μg ml,峰面积与其含量呈良好的线性关系。 结论 :该法操作简便、快速、准确 ,为组织中单胺类递质及其代谢产物检测的一种理想方法 ,并适用于临床相关研究。     

川芎挥发油化学成分研究

采取闪蒸气相毛细管色谱法和气相毛细管色谱—质谱法研究了宁夏六盘山区产川芎的挥发油化学成分,色谱分离出50多个峰,质谱鉴定了24个成分,主要是川芎酜内酯(46.37％)、丁基酞内酯(13.87％)、新蛇床内酯(6.98％)和丁烯基酜酯(4.8％)。红外光谱图中有较强的内酯特征吸收峰,为质谱所鉴定的以上主要成分提供了佐证。将闪蒸气相色谱法与蒸气蒸馏提取气相色谱法进行对照,二者的色谱图基本相符,前者是分析天然产物挥发性成分更加简便、迅速的微量方法。     

气相色谱用于肠通透性监测的研究

作者采用国产气相色谱及９２０２微机数据处理系统，对临床患者和实验动物肠通透性改变进行监测。该方法以甘露醇（Ｍ）和乳果糖（Ｌ）为探针，用气相色谱检测尿中糖分泌率及Ｌ／Ｍ比值。结果显示，测定标准品Ｍ和Ｌ随进样量增加而呈线性改变，与国外学者报道一致。比较不同浓度进口与国产乳果糖，证明二者在研究肠通透性方面高度相关（ｒ＝０．９９）。检测急性胰腺炎并发感染动物的尿标本，发现乳果糖大量排出，Ｌ／Ｍ值明显增加。作者认为，气相色谱为一行之有效的方法用于肠通透性监测，有助于临床上对内源性感染及脓毒症的早期诊断。     

血液灌流对硫线磷和硫酸阿托品的吸附作用

目的 定量研究血液灌流对有机磷农药硫线磷和其解毒药阿托品的吸附作用.方法 模拟临床血液灌流装置,对含硫线磷和硫酸阿托品的血样进行灌流吸附,分别用毛细管气相色谱法和高效液相色谱法测定硫线磷和硫酸阿托品的残留量.结果 吸附剂用量为0.5、1.0和1.5 g,包膜活性炭在灌流2.0 h后硫线磷的清除率均能达到90%以上,硫酸阿托品的清除率依次为61.9%、84.9%和88.9%;HA230树脂在灌流1.5 h后硫线磷清除率都达到90%以上,硫酸阿托品的清除率也依次高达88.0%、97.2%和98.4%;包膜活性炭灌流3.0h后,硫酸阿托品与硫线磷的比值最高为灌流前的10.1倍,而HA230树脂灌流后,此比值最高为灌流前的6.7倍.结论 包膜活性炭和HA230吸附树脂血液灌流1.5～2.0 h均能清除血中大部分硫线磷,而且均能增加血中硫酸阿托品和硫线磷浓度的比值.     

Analytical studies on illicit heroin

The recovery of heroin in fumes was investigated. In the Netherlands the common mode of heroin smoking is the chasing the dragon procedure: heroin is heated on an aluminium foil by a lighter and the fumes are inhaled. The efficiency of the volatilization of heroin using this procedure was studied under laboratory conditions using thin layer chromatography, gas chromatography and high pressure liquid chromatography. A considerable influence of the form (salt or base) of the heroin was found as well as strong influences of other substances that may be present in illicit heroin samples as diluents. The danger of the inhalation of fumes containing unknown pyrolysis products is mentioned and a hypothesis is given for the phenomenon of heroin-leucoencephalopathy that was observed in heroin smokers in Amsterdam in 1981. The types of heroin encountered in the Netherlands are discussed with regard to their suitability for smoking.     

NAD-Sepharose 6MB亲和胶的制备及在2,5-二酮基-D-葡萄糖酸还原酶纯化中的应用

目的制备NAD亲和胶,用于分离纯化2,5-二酮基-D-葡萄糖酸还原酶。方法将NAD通过丁二酸二酰肼与溴化氰活化的Sepharose6MB胶联结,制得NAD亲和胶。从棒杆菌细胞中提取的2,5-二酮基-D-葡萄糖酸还原酶粗酶液用NAD亲和胶进行亲和层析纯化。结果NAD的结合率为71．67％;亲和层析回收率为77．27％;酶的比活提高了1．1倍。结论以NAD为配基的亲和胶用于纯化以NADPH为辅酶的2,5-DKG还原酶行之有效。     

分清五淋丸的薄层色谱鉴别

目的寻找控制分清五淋丸质量的方法。方法利用薄层色谱对其中大黄、黄柏、黄芩和栀子4种主药进行检出研究。结果样品不仅与黄连素、黄芩素和栀子甙对照品有一致的层析斑点,且与对照药材有一致或基本一致的层析斑点。结论薄层色谱方法是控制分清五淋丸质量的有效方法。     

Role of inter-α-inhibitor and its related proteins in urolithiasis. Purification of an inter-α-inhibitor related protein from the bovine kidney

Urine contains several macromolecules that inhibit calcium oxalate (CaOx) crystallization. Among them is bikunin, the light chain of most of the inter-α-inhibitor (IαI) family of glycoproteins. This study aimed to verify whether bikunin and other members of the IαI family are synthesized in the kidneys or derived exclusively from the plasma. Proteins extracted from homogenized bovine kidney were applied successively to three chromatographic steps on DEAE-Sephacel, Sephacryl S-300, and Mono Q column. The inhibitory activity was assayed using a CaOx crystallization system. The presence of IαI-related proteins was determined by␣electrophoresis and Western blotting. The results showed that kidney extract contained a 125-kDa protein that cross-reacted with anti-IαI antibodies. This protein inhibited CaOx crystallization efficiently. According to its molecular weight and immunoreaction with anti-IαI antibody, the 125-kDa protein could be pre-α-inhibitor. The latter is known to encompass a heavy chain and bikunin, which may explain its inhibitory activity against CaOx crystallization. Consequently, we hypothesize that kidneys may produce some IαI-related proteins that are involved in the inhibition of stone formation. Received: 18 February 1998 / Accepted: 9 July 1998     

梦宁片中栀子苷的稳定性研究

目的 建立梦宁片中栀子苷含量的HPLC测定方法,并以此考察栀子苷的热稳定性,为确定梦宁片的有效期提供动力学数据。方法 超声提取样品,流动相:0.2％三乙胺水溶液(含0.1％磷酸)-乙腈(85:15):检测波长240 nm;流速:1.0 mL·min~(-1)。采用高温加速试验法对栀子苷的热稳定性进行研究。结果 栀子苷在0.10μg～0.52μg的范围内线性关系良好,相关系数r=0.9997;平均回收率为98.92％,RSD=2.81％(n:5);该复方中栀子苷的变化为一级反应,常温下梦宁片以栀子苷为指标的有效期为2.83年。结论 该方法的建立对快速确定药品的有效期,缩短新药的开发周期具有实际意义。     

骨疏灵胶囊的质量标准研究

目的：研究骨疏灵胶囊的质量控制标准。方法：采用薄层色谱法对制剂中的补骨脂、女贞子进行定性鉴别；并利用高效液相色谱法对制剂中的淫羊藿苷进行定量分析，以CH3CN-H2O(30：70)为流动相，流速1．0mL／min，色谱柱为C18柱，检测波长为270nm。结果：补骨脂与女贞子的薄层色谱鉴别专属性强，阴性对照无干扰；淫羊藿苷在0.0968～0.4840μgg范围内线性关系良好(r=0．9999)，平均回收率为97．27％(RSD=1．88％，n=5)。结论：该方法可为骨疏灵胶囊的质量评价提供科学依据。