载药脂质体包封率测定方法的研究进展

载药脂质体已经成为改善药物体内行为或实现靶向给药的重要新剂型,对其关键工艺过程和相应的关键质量属性进行研究和控制是载药脂质体研究的重要工作.包封程度的高低直接决定药物在体内的疗效,因此,包封率是脂质体的关键质量属性之一.本文对常用的包封率测定方法及其特点进行分析与比较,探讨了包封率测定时需考虑的主要因素,为载药脂质体剂...     

香附化学成分研究

目的 研究莎草Cyper us rotundus根茎(香附)的化学成分.方法 采用硅胶、Sephadex LH-20等色谱方法对香附根茎中的化学成分进行分离纯化,应用谱学技术和化学方法鉴定化合物的结构.结果 从香附药材中分离得到10个化合物,分别鉴定为5,7,4 ′-三羟基-2′-甲氧基-3′-异戊烯基异黄酮(1)、6-O-p-hydroxybenzoyl-6-epi-aucubin(2)、6-O-p-hydroxybenzoyl-6-epi-monomelittoside (3)、verproside (4)、syringopicroside B(5)、syringopicroside C(6)、oleuropeinic acid (7)、oleuroside (8)、10-hydroxyoleuropein (9)、senburiside Ⅰ (10).结论 化合物1为新化合物,命名为香附酮A,化合物2～10为首次从该植物中分离得到.     

Sephadex G-10凝胶色谱系统测定头孢西丁钠中高分子聚合物

目的:建立测定头孢西丁钠中高分子聚合物的含量.方法采用Sephadex G-10凝胶色谱系统.色谱柱:葡聚糖凝胶G-10色谱柱;流动相A:pH 7.0的0.1 mol·L-1磷酸盐缓冲液[0.1 mol·L-1磷酸氢二钠溶液-0.1 mol·L-1磷酸二氢钠溶液(61:39)],流动相B:超纯水;流速:1.0 mL·min-1,检测波长:254 nm.结果:头孢西丁钠高分子聚合物在5～70 g·L-1的范围内线性关系良好,r=0.994 3.结论:本方法专属性强,准确度高、重现性好,可作为头孢西丁钠中高分子聚合物含量的测定方法.     

猪卵透明带的分离和提纯

用机械方法绞碎猪卵巢,经不同孔径尼龙筛过滤及热溶解等方法取得的去卵母细胞透明带,用双向-SDS-聚丙烯酰胺凝胶电泳(简称2D-PAGE)后,不论用考马斯蓝染色或银染色,均得两条分子量分别为74000～102000和98000～118000的条带,称为ZP_1和ZP_2。 将去卵母细胞的透明带用葡聚糖凝胶(Sephadex)G-100柱层析分离,得到A和B两个吸收峰,用2D-PAGE分析,证实A峰内仍含有ZP_1及ZP_2抗原,而B峰内为一些其他蛋白的染色点,提示Sephadex柱层析可进一步纯化透明带抗原。     

葡聚糖凝胶色谱法分析注射用阿洛西林钠中的高聚物

目的建立一个简单分析阿洛西林钠中高聚物的方法。方法采用Sephadex TM G-10色谱柱,以0．1mol·L-1磷酸盐缓,中液（氢氧化钠调pH6．8）为流动相A,水为流动相B,流速1．5mL·min-1,检测波长为254nm。结果阿洛西林钠中高聚物在0．001～4．08mg·mL-1内线性关系良好,检测限为0．5ug·mL-1。当供试品溶解量为200mg·mL-1时,本法的高聚物检出能力达到百万分之三。结论所用方法简便,结果可靠,可用于阿洛西林钠中高聚物的检测。     

以Sephadex G-100制备微柱凝胶血型卡及其性能评估

目的本实验以Sephadex G-100制备血型卡并对其进行性能评估。方法用生理盐水浸泡等对Sephadex G-100凝胶进行预处理,通过控制浸泡时间、缓冲液、加入红细胞的量及其浊度等,制备血型卡。再对血型卡进行性能评估,包括符合率、灵敏度、批内重复率、批间重复性、有效期等。结果自制血型卡检测200例标本的血型结果和试管法、强生血型卡法全部符合。自制血型卡和强生凝胶卡检测抗B抗体平均滴度均为1:308,均明显优于传统试管法1:256(P<0.05)。自制血型卡检测抗B抗体滴度的批内重复性CV为8.1%,批间重复性CV为3.7%。自制血型卡稳定期约为8个月。结论以Sephadex G-100凝胶试剂制备血型卡具有重复性高、稳定性好、结果准确、试剂制备工艺简单、成本低等优点,具有较好的推广应用和开发价值。     

藏药甘松多糖S的研究

目的 对甘松多糖S（Nardostachys chinensis polysaccharide S,NCPS）的组成进行研究。方法 采用水提醇沉法提取甘松多糖粗品,并通过乙醇分级沉淀,Sevage法除蛋白,葡聚糖凝胶柱色谱纯化;UV和IR等方法考察多糖性质,凝胶渗透色谱-示差检测法测定多糖的纯度和相对分子质量范围及分布,HPLC法鉴定单糖组成及其物质的量比值。结果 得到一种淡黄色粉末NCPS。紫外光谱分析在195 nm波长处有明显吸收峰,在260、280 nm等处无吸收峰,表明被测物为多糖,且不含核酸及蛋白质;红外吸收光谱分析,在3 412.15、2 934.10、1 642.11、1 438.96、1 242.67、1 103.54、830.86、636.12 cm^?1等处均有明显的多糖的特征吸收;其重均相对分子质量为7 082;NCPS主要由阿拉伯糖、木糖、果糖和葡萄糖组成,其物质的量的比值为0.69∶1.0∶3.92∶2.28。结论 NCPS为一种杂多糖,首次从甘松中分离得到。     

川芎嗪长循环脂质体包封率的测定

目的建立川芎嗪长循环脂质体的包封率测定方法。方法采用葡聚糖凝胶-G50微型柱分离脂质体和游离药物,以高效液相色谱法分别测定含量,并计算包封率。结果葡聚糖凝胶-G50可使川芎嗪长循环脂质体和游离药物完全分离;HPLC条件下,川芎嗪与辅料和溶剂峰分离良好,川芎嗪浓度在1．09～43．60[zg／mL范围内线性关系良好（r=0．9994,n=6）。结论所建立的方法简单可行、重复性好、准确、稳定,为评价和控制川芎嗪长循环脂质体的质量提供了依据。     

Effect of swim-up, Percoll and Sephadex sperm separation methods on the hypo-osmotic swelling test.

The separation of spermatozoa from the seminal plasma is required to prepare the spermatozoa for intrauterine insemination, in-vitro fertilization and sex selection. This study evaluated the effects of sperm preparation techniques on the functional integrity of the sperm membrane, as measured by the hypo-osmotic swelling test (HOS). Thirty-four semen specimens obtained from the male partner of infertile couples were evaluated. A semen analysis and HOS test were performed on each specimen. The remainder of the specimen was divided into three equal aliquots, the first prepared using Percoll, the second using a swim-up method and the third using a Sephadex column. After the preparation, a semen analysis and HOS test was performed on each aliquot. The mean and standard deviation for the HOS test was 72.9 +/- 8.5% initially, 71.2 +/- 13.1 after Percoll, 75.2 +/- 15.1 after swim-up and 62.4 +/- 14.5 after Sephadex. Analysis of variance showed that the mean HOS score was the same after Percoll and swim-up as it was initially but significantly lower after preparation with Sephadex. There was also a higher proportion of abnormal semen specimens (HOS less than 50%) after preparation with Sephadex than after the other preparation methods. We recommend the use of the HOS test as part of a screening panel for sperm separation.     

Synthesis of glycosaminoglycans and other macromolecules by embryo calf epiphyseal cells in culture

Monolayer cell cultures from the distal femoral epiphyses of embryo calves were studied following the first subculture, which was carried out after confluence in primary culture. Light microscopic examination revealed scattered deposits of metachromatic-staining material; on electron microscopy fine fibrils considered to be developmental collagen were seen. After several days in culture lacuna-like patterns of cells were seen. The nature of the cell secretions were studied by radioactive precursors, which were fractionated on Sephadex G200 and by ion exchange chromatography. Enzyme digestion with bacterial and testicular hyaluronidase and chondroitinase-AC and-ABC revealed that the cells synthesized 70% sulphated, and 30% non-sulphated glycosaminoglycans. Of the sulphated glycosaminoglycans 70% was chondroitin-4-sulphate, 20% chondroitin-6-sulphate, and the remainder probably keratansulphate. Studies were labelled amino acid precursors suggested that the cells synthesized a high-molecular weight protein containing hydroxyproline, as well as some non-collagenous protein, shown by tryptophan incorporationThis work was reported in part at the Second Australian Symposium on Calcium and Calcified Tissue Metabolism, in Melbourne, Australia, August 14th–15th, see Calc. Tiss. Res.4, 274–290 (1969).