安宫牛黄丸体外安全性评价方法的研究

研究安宫牛黄丸中可溶性汞及三种毒性汞价态的体外溶出检测方法,探讨安宫牛黄丸体外安全性评价方法。通过试验研究提取溶剂、净化方式、提取、净化时间等因素对溶出的影响,确定最佳的提取方案。使用电感耦合等离子体质谱法测定可溶性汞,高效液相色谱法-电感耦合等离子体质谱法联用测定三种汞价态。安宫牛黄丸中可溶性汞及三种毒性汞价态的最佳提取方法为：用人工肠液在37 ℃下超声处理2 h,提取液静置20 h后取上清液。方法重现性好,最大程度地模拟药物在体内的吸收环境。安宫牛黄丸提取液中可溶性汞含量较高,但不含汞的有毒价态：甲基汞、乙基汞和二价汞。该方法可推广应用于含朱砂中成药中可溶性汞及其价态的体外溶出和测定。以毒性大的三种汞价态：甲基汞、乙基汞和二价汞作为体外指标,可在一定程度上评价安宫牛黄丸的安全性。     

甘草苷在玻碳电极上的电化学行为及其测定

在pH 3.00的B-R缓冲溶液中,采用差分脉冲伏安法(DPV)、线性扫描伏安法(LSV)和循环伏安法(CV)研究了甘草苷在玻碳电极上的电化学行为, 建立了测定甘草苷的DPV法。实验结果表明,甘草苷于1.16 V (vs.Ag/AgCl)处产生一个氧化峰,峰电流和甘草苷的浓度在2.00×10-6~3.50×10-5 mol/L范围内呈良好的线性关系,检出限为8.25×10-7 mol/L。该法用于实际样品甘草、胃康灵和逍遥丸中黄酮含量的测定(以甘草苷为对照品),平均回收率分别为97.1%、98.9%和102.0%。此外对电极反应机理作了初步探讨。     

原子吸收法建立舒筋活血中成药的无机元素的控制方法的探讨

人们已认识到无机元素与中成药的疗效有密切相关。但是在研究舒筋活血中成药化学成分的质量控制时, 无机成分常被忽视。 文章用原子吸收光谱法,测定了中成药大活络丸和几种中药中15种无机元素Cu, Ca, Fe, K, Mg, Mo, Ni, Sr, V, Mn, Zn, Na, Cr, Cd和Hg的含量, 探讨了无机元素与中药的药效关系,并通过大活络丸与几种中药所含无机元素含量的对照比较, 得出大活络丸中Fe, Cu, Mn和Zn等与药效之间的关系。中成药大活络丸中所含一定量的Fe, Cu, Mn和Zn等微量元素与其祛风除湿,理气豁痰,舒筋活络等药效存在一定关联。对大活络丸的无机元素测定与分析可为今后其指纹图谱的建立提供数据和参考依据。     

正相模式/反相模式的二维液相色谱系统的构建与应用

以4.6mm×50 mm i. d.的Hypersil SiO2正相色谱柱为第一维,4.6mm×250 mm i. d.的Kromasil C18反相色谱柱为第二维,通过升高第二维色谱温度的方法增加两维流动相间互溶性的方法构建了定量环-阀切换接口的二维液相色谱系统(NPLC×RPLC)。根据有机溶剂的特征,在第一维正相色谱流动相中加入二氧六环;第二维反相色谱流动相中加入异丙醇,在改善流动相兼容性的同时,有效调整分离选择性。采用此系统对正天丸样品进行分离分析,达到1120的峰容量。     

中成药速效救心丸的红外光谱聚类分析研究

对同一厂家同一批号和不同批号的速效救心丸的红外图谱进行了测定,对影响红外光谱测定的实验条件包括粒度和混合比例进行了优化选择。实验结果表明,该方法具有很好的精密度、重复性和稳定性;采用模式识别中的聚类分析,对同一批号和不同批号的速效救心丸进行了分析比较,结果表明,同一批号的速效救心丸样本的红外图谱具有良好的重复性,当相关系数达到0.992时,所分析的60个样本聚为一类,说明该厂家同一批号及不同批号速效救心丸的产品质量具有较好的稳定性,红外光谱法结合聚类分析法可以简便快速地完成对中成药制剂的质量评价。     

Na(4D)+Na(3S)Na(4F)+Na(3S)碰撞能量转移截面

利用双光子吸收,将Na(3S)原子激发到4D态,测量了Na(4D)+Na(3S)Na(4F)+Na(3S)碰撞能量转移截面,因为直接由4F→3D的荧光不能探测,所以检测3D→3P级联荧光讯号。结合基态钠原子密度的测量,给出了截面值σ_4D→4F=1.3 x 10~(-14)±28％(cm~2)。     

Rapid discovery of absorbed constituents and metabolites in rat plasma after the oral administration of Zi Shen Wan using high‐throughput UHPLC–MS with a multivariate analysis approach

Zi Shen Wan is a typical formula consisting of three herbs, Phellodendri Amurensis Cortex, Rhizoma Anemarrhenae, and Cortex Cinnamomi, and has been widely used for treating prostatitis and infection diseases. However, it lacks in‐depth research of the constituents of Zi Shen Wan in vivo and in vitro. In this work, ultra high performance liquid chromatography coupled with quadrupole‐time‐of‐flight mass spectrometry and MassLynx software was established to characterize the chemical compositions of Zi Shen Wan in vivo and in vitro. In total, 92 peaks were characterized in vitro and 33 peaks were characterized in vivo based on mass spectrometry and tandem mass spectrometry data. Among the 33 compounds characterized in rat plasma, 22 prototype components absorbed in rat serum and 11 metabolites were identified in vivo. This work was fully reports the chemical constituents of traditional Chinese formula of Zi Shen Wan, it demonstrated that ultra high performance liquid chromatography combined with quadrupole time‐of‐flight mass spectrometry coupled to MassLynx software and multivariate data processing approach could be successfully applied for rapid screening and comprehensive analysis of chemical constituents in vitro and prototype components or metabolites in vivo of traditional Chinese medicine.     

Extraction of paeonol from Jisheng Shenqi Wan using supercritical fluid extraction

Supercritical carbon dioxide with or without methanol and 95% ethanol modifiers was used to extract paeonol from the pills of Jisheng Shenqi Wan and high-performance liquid chromatography (HPLC) was used to analyze the extract. The effect of temperature and pressure on the yield of paeonol was tested. The results show that the recovery of paeonol was improved by adding a polar modifier, such as methanol and 95% ethanol in supercritical fluid. The yield obtained after 120 min extraction with 95% ethanol modified-supercritical carbon dioxide was the highest (1.51, w/w at 60 degrees C and 400 bar), while that obtained with supercritical carbon dioxide only at 40 degrees C was the lowest from 0.67 to 0.83 over a range of 200-600 bar.     

Analysis and Identification of the Chemical Constituents of Ding‐Zhi‐Xiao‐Wan Prescription by HPLC‐IT‐MSn and HPLC‐Q‐TOF‐MS

Ding‐Zhi‐Xiao‐Wan (DZXW) is a famous traditional Chinese medicine (TCM) formula, which is composed of four herbs, Ginseng Radix, Poria, Polygala Radix and Acori Tatarinowii Rhizoma. It has been popularly used for the treatment of emotional disease, like Alzheimer's disease, Parkinson's disease, depression, anxiety, forgetfulness and neurasthenia. In this research, a high‐performance liquid chromatography coupled with ion‐trap tandem mass spectrometry (HPLC‐IT‐MSⁿ) method along with a high‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry (HPLC‐Q‐TOF‐MS) method in negative ion mode was established to investigate the major constitutions in DZXW. The extracts were prepared by ultra‐sonication in ethyl acetate, n‐butanol, 95% ethanol and deionized water sequentially as well as in deionized water directly. A Kromasil C18 column was used to separate the extracts of DZXW. Acetonitrile and 0.1% aqueous formic acid (V/V) were used as the mobile phase. A total of 64 components were characterized, including 16 triterpenoids, 14 Polygala saponins, 10 oligosaccharide esters, 6 sucrose esters, 2 xanthone C‐glycosides and 16 ginsenosides.     

乌鸡白凤丸及其制剂中微量元素的研究

以前用化学计量法的聚类分析法,对乌鸡白凤丸等中成药进行过研究。发现十二乌鸡白凤丸(南方方剂)与乌鸡白凤丸(北方方剂)中微量元素的聚类分析结果不是在同一群组,差异较大。采用原子吸收光谱法,对十二乌鸡白凤丸与乌鸡白凤丸及其制剂泰和武山乌鸡与土鸡中微量元素进行测定,并进行研究。结果表明：十二乌鸡白凤丸与乌鸡白凤丸中微量元素差异大。而泰和武山乌鸡与土鸡中微量元素差异不大。十二乌鸡白凤丸与乌鸡白凤丸中差异大的原因不在其制剂乌鸡,而在其他药中。