基于指纹图谱分析和多成分同时定量的益安宁丸质量评价研究

摘 要 目的：建立益安宁丸的HPLC指纹图谱,并测定5种主要成分（人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1、五味子酯甲和丹参酮ⅡA）的含量,为益安宁丸的质量控制提供可靠方法。 方法: 采用Waters Sunfire TM C18色谱柱（250 mm×4.6 mm,5 μm）,以乙腈（A） 0.1%磷酸水溶液（B）为流动相,梯度洗脱（0～5 min,2% A;5～15 min,2%A→10%A;15～25 min,10%A→30%A;25～40 min,30% A;40～60 min,30% A→90% A;60～70 min,90% A）;流速为1.0 ml·min-1;检测波长为203 min（0～60 min,检测人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1和五味子酯甲）、270 nm（60～70 min,检测丹参酮ⅡA）;柱温35 ℃。 结果: 在指纹图谱研究中,共确定益安宁丸HPLC指纹图谱26个共有峰,通过与混合对照品比较指认其中7个指标成分,分别是6号 五味子酯甲、16号 人参皂苷Rg1、17号 人参皂苷Rb1、18号 三七皂苷R1、23号 丹参酮Ⅰ、24号 五味子甲素和26号 丹参酮ⅡA,利用相似度软件对14批样品指纹图谱进行分析,各批样品相似度均在0.98以上。在建立的色谱条件下试验5个成分分离度良好,方法精密度和重复性RSD值均＜1.5%,供试品溶液在24 h内稳定,各成分具有良好的线性关系和较宽线性范围;6批益安宁丸中人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1、五味子酯甲和丹参酮ⅡA质量分数分别在7.187 0～7.254 0,9.086 0～9.250 0,2.109 0～2.288 0,11.208 0～11.338 0和1.374 0～1.458 0 mg·g-1。 结论: 所建立的益安宁丸HPLC指纹图谱检测和定量测定分析方法快速、准确,可以有效地评价益安宁丸的质量。     

抗生素西索米星发酵过程中次要组分的调控

在西索米星产生菌橄榄星孢小单孢菌Ｍ－４１的发酵代谢与产物合成的研究中,发现通过控制种子期菌丝的生长形态、培养基中磷酸盐含量,并在发酵过程中添加合适的抑制剂,可有效地减少发酵液中次要组分ｖｅｒｄａｍｉｃｉｎ的生物合成,增加主要组分西索米星的含量。     

Preparation of bovine serum albumin loaded poly (D,L-lactic-co-glycolic acid) microspheres by a modified phase separation technique

BSA-loaded mcirospheres were prepared by a modified phase separation method, in which petroleum ether (PE) containing a certain amount of Span 80 rather than poly (dimethylsiloxane) (PDMS) was adopted as coacervating agent. Process parameters such as Span 80 concentration, the volume and addition rate of coacervating agent, polymer concentration, agitation rate during the phase separation process and PE type were evaluated to optimize the protein encapsulation. It was found microspheres with high yield (>80.0%) and entrapment efficiency (>90%) could be obtained using PE containing 5.0% Span 80 as the coacervating agent. Microspheres with small particle size (<10?µm) could be produced successfully with appropriate process parameters. In vitro release study suggested that burst release was significantly influenced by Span 80 concentration, polymer concentration and PE type and the burst release could be reduced to <20% with optimized formulation. A biphasic release behavior in vitro test was observed for the microspheres prepared by this method. GC analysis demonstrated that residual solvent of DCM and petroleum ether was decreased dramatically in comparison with PDMS used as a conventional coacervating agent.     

加兰他敏治疗阿尔茨海默病作用机制的研究进展

阿尔茨海默病是老年性痴呆中最常见的一种类型。加兰他敏作为第二代乙酰胆碱酯酶抑制剂，原用于治疗重症肌无力和小儿麻痹后遗症等疾病，近年来被应用于临床治疗阿尔茨海默病．效果明显。本文就加兰他敏治疗阿尔茨海默病作用机制的最新研究情况作一简要概述。     

喷他佐辛压敏胶分散型贴剂的制备研究

目的研制喷他佐辛压敏胶分散型贴剂并考察其体外经皮渗透性。方法将喷他佐辛及各种促渗剂直接溶于压敏胶中制备压敏胶分散型贴剂,采用卧式双室扩散池,研究其体外经皮渗透行为。结果由Duro-Tak 87-9301型压敏胶制备的贴剂具有较好的稳态渗透速率。5%氮酮与10%豆蔻酸异丙酯合用对喷他佐辛促渗效果明显,经皮渗透速率为(11.28±0.63)μg/(cm2.h),促渗倍率达3.01倍。贴剂中喷他佐辛的含量由2%增加到4%,经皮渗透速率明显增大,含量增加到6%和8%时渗透速率无明显变化。结论所得处方中各因素的组合有利于喷他佐辛的经皮吸收。     

基体辅助激光解吸质谱法在生物大分子质量研究中的应用

研究了基体辅助激光解析飞行时间质谱法(MALDI-TOF MS)测定蛋白和糖蛋白的实验条件,实测了重组人白细胞介素2、肿瘤坏死因子、粒细胞巨噬细胞集落刺激因子、白细胞干扰素α2b、白细胞干扰素α₁、促红细胞生成素、钙调蛋白及其片段、大鼠脑型一氧化氮合成酶和天然牛精液蛋白提取物的分子量和纯度,鉴定了蛋白质混合物中各单个成分,结果表明MALDI-TOF MS可有效地研究基因工程蛋白质和天然蛋白提取物等生物大分子的质量。     

高效液相色谱法测定金钱草胶囊中槲皮素的血药浓度

目的建立金钱草胶囊中槲皮素的血药浓度测定方法,为临床应用和药代动力学研究提供技术参考。方法采用高效液相色谱-紫外检测方法测定,色谱柱为Kromasil C8柱(250 mm×4.6 mm,5μm),流动相为甲醇-乙腈-0.4%磷酸溶液(40∶10∶50),流速1 mL/min,柱温30℃,进样量20μL,检测波长360 nm。血样提取方法,以β-葡萄糖苷酸酶水解后,以乙酸乙酯提取,氮气流吹干后复溶进样。结果槲皮素保留时间约为8.8 min,金钱草胶囊中槲皮素的血药浓度线性范围0.08～12μg/mL,最低定量限为0.05μg/mL,检测限为0.02μg/mL。方法平均回收率为97.50%～102.50%,水解提取回收率为76.46%～87.43%,日内精密度RSD为4.18%～6.17%,日间精密度RSD为5.08%～8.63%。结论方法简便,分析速度快,灵敏度较高,重复性好,适用于临床血药浓度测定及药代动力学研究。     

注射用促肝细胞生长素辅料的研究

寻找一种注射用促肝细胞生长素（ＨＧＦ）适用的辅料。方法：以三批不同批次的ＨＧＦ原料液为实验对象,分别通过 Ｆｏｌｉｎ－酚和~３Ｈ－ＴｄＲ掺入法研究了三种辅料： ３％右旋糖酐, ８％甘露醇, ２％右旋糖酐＋ ８％甘露醇对ＨＧＦ多肽含量及活性的影响。结果：８％甘露醇作为辅料时使ＨＧＦ多肽含量测定显著增高,而右旋糖酐则不影响测定结果。三种辅料对ＨＧＦ活性均无显著影响。结论：最终选用３％右旋糖酐作为ＨＧＦ的辅料。     

A novel approach to prepare tripolyphosphate/chitosan complex beads for controlled release drug delivery

A novel approach was developed to improve the mechanical strength of tripolyphosphate (TPP)/chitosan beads prepared under coagulation condition at 4 degrees C in the presence of gelatin. Cross-sectional analysis indicated that the beads had a homogeneous crosslinked structure, as a result the beads were strengthened greatly (the mechanical strength increased more than ten times). Furthermore sodium alginate (a polyanion) can interact with cationic chitosan on the surface of these TPP/chitosan beads to form polyelectrolyte complex film for the improvement of the drug sustained release performances. The loading efficiency of model drugs (brilliant blue and FITC-dextran) in these beads was very high (more than 90%). Crosslinking time, TPP solution pH and other preparation factors had an effect on the drug release performance of beads. The release period of brilliant blue (a poor water soluble dye) was more than 2-months at a fairly constant rate in 0.9% NaCl, 10 mM PBS pH 7.4. However, for FITC-dextran (a water soluble polysaccharide) only 1-2 days in the same conditions. It seems that TPP/chitosan bead prepared by the novel method is a promising formulation for drug delivery.