高锰酸钾-甲醛-多巴酚丁胺化学发光体系的研究

在酸性条件下,盐酸多巴酚丁胺与高锰酸钾能够产生微弱化学发光,而甲醛能够大大地增强该发光.在一定条件下,发光强度与多巴酚丁胺的浓度呈良好的线性关系.由此并结合流动注射分析技术,建立了一种测定多巴酚丁胺的新方法.方法的检出限为8 7×10-9g/mL(IUPAC),线性范围为1 0×10-8～1 0×10-6g/mL,对1 0×10-7g/mL多巴酚丁胺平行测定11次,其相对标准偏差为2 3%.     

SDS和PCN与胶束中NRa的相互作用

检测体系的紫外可见光谱、荧光光谱、表面张力、电导率等,研究了十二烷基硫酸钠(SDS)和盐酸普鲁卡因(PCN)与酸性形态中性红(NRa)的相互作用.中性红能降低SDS的临界胶束浓度.在SDS稀溶液中,表面活性剂分子能减弱NRa紫外吸收光谱及荧光发射光谱的强度.随着SDS溶液浓度的增大,NRa的光谱强度增大.NRa吸附于球状胶束表面,定位于棒状胶束膜相较深处.在SDS胶束体系中,随着PCN的加入,NRa的紫外可见光谱、荧光光谱强度减弱.     

氨噻肟酸-锅法合成头孢吡肟盐酸盐

以氨噻肟酸为原料与二乙氧基硫代磷酰氯反应合成新活性酯溶液,直接与(6R,7R)-7-氨基-3-[(1-甲基-1-吡咯烷)甲基]头孢-3-烯-4-羧酸盐酸盐(7-Acp)在混合溶剂中反应得到头孢吡肟盐酸盐一水合物,该合成方法产率高、质量好、成本低,适合于生产。     

盐酸丙帕他莫的合成和结构表征

盐酸丙帕他莫为一种非成瘾性镇痛药.以对乙酰基氨基酚为起始原料,经酰化、胺解、酸化成盐得到盐酸丙帕他莫.通过元素分析、UV、IR、1H NM R和M S对结构进行表征.改进后的工艺总收率达68.8%(以对乙酰基氨基酚计).结果表明操作方法简便,总收率较高。     

诃子中盐酸小檗碱的提取方法研究

采用两种不同方法提取了蒙药材诃子中盐酸小檗碱,用分光光度法测定其含量,检测波长426 nm.结果显示,在0 mg/ml-0.4 mg/ml范围内,服从郎泊-比尔定律,平均回收率分别为96.51%和96.65%,超声波辅助萃取法简便快速.     

用HPLC法同时测定可立停中的愈创木酚甘油醚、马来酸氯苯那敏和盐酸甲基麻黄碱

建立了同时测定可立停中的愈创木酚甘油醚、马来酸氯苯那敏和盐酸甲基麻黄碱含量的高效液相色谱法。色谱条件:以Shim-pack CLC-ODS 150mm×6.0mm为分析柱,以甲醇:水:三乙胺=40:60:0.2(水相用H_3PO_4调节到pH=3.0)溶液为流动相,检测波长为220 nm。结果表明,测定念创木酚甘油醚的线性范围为0.24～1.92mg/mL,平均回收率为99.86％,RSD=0.33％;测定马来酸氯苯那敏的线性范围为0.0072～0.057 6 mg/mL,平均回收率为99.77％,RSD=2.58％,测定盐酸甲基麻黄碱的线性范围为0.04～0.32mg/mL,平均回收率为95.83％,RSD=2.79％。     

Unfolding of C2A Domain of Synaptotagmin I in the Presence of Guanidine Hydrochloride

The C2 domain originally referred to the second of four constant structural motifs in protein kinase C (PKC). Now this domain represents a large structural family sharing a homologous dimensional structure in many proteins that play important roles in many organisms. The C2A domain is one of the two C2 domains of synaptotagmin I involved in the Ca^2 regulation of exocytosis. This domain is mostly composed of β-sheet except for a small fraction of α-helix, and therefore provides an ideal model for a protein folding study. In this report, the unfolding equilibrium of the C2A domain in guanidine hydrochloride (GdnHCI) containing solutions has been studied using ultraviolet (UV) difference spectrum, fluorescence spectrum, size exclusion chromatography (SEC), and circular dichroism (CD) spectrum. The results suggest that unfolding of the C2A domain occurs as a two-state process during GdnHCI titration. By examining the changes of both tertiary structure and secondary structure, no intermediates could be detected during this unfolding study. However, it has been found that the native state of the C2A domain has a large hydrophobic surface. This result suggests that as a fragment of a protein, the C2A domain itself may exist in a state with large hydrophobic surface. This hydrophobic surface may be the molecular basis for interaction between domains in the whole protein.Furthermore, the hydrophobic behavior may play a role during the oligomerization of svnaptotagmin.     

高效液相色谱法测定盐酸托烷司琼片的含量

建立高效液相色谱法测定盐酸托烷司琼片含量,采用Zorbax SB-C18色谱柱(4.6 mm×150 mm,5μm),流动相为0.02mol.L-1磷酸二氢钾溶液(稀氢氧化钾溶液调节至pH5.5)-甲醇-乙腈(35∶40∶25),流速0.8 mL.min-1,检测波长为285 nm。进样量在0.25～3.0μg时,与峰面积比值呈良好线性,r=0.999 9(n=7),平均回收率100.1%,日内和日间RSD分别为0.30%及0.36%(n=9)。该法简便、准确、专属,可用于该片的质量控制。     

盐酸托烷司琼片溶出度方法的研究

建立盐酸托烷司琼片溶出度测定法,以0.01 mol/L盐酸溶液为溶出介质,浆法,转速50 r.min-1,检测波长为285nm。盐酸托烷司琼浓度在2.0～24.0μg.mL-1时,与峰面积比值呈良好线性,r=0.999 9(n=7),平均回收率100.2%,日内和日间RSD分别为0.62%及0.80%(n=9)。该法简便、准确,可用于该片的质量控制。     

盐酸倍他洛尔片溶出度测定方法研究

建立了盐酸倍他洛尔片溶出度的UV测定方法,并研究了盐酸倍他洛尔片的溶出曲线.UV检测波长为274 nm,线性范围为40~140 mg.L-1,相关系数r=0.999 8;平均加样回收率为99.91%,RSD为0.35%;连续进样精密度8、h溶液稳定性的RSD分别为0.02%、0.04%.该方法简便、快速、准确度高.