t检验法用于评价中药色谱指纹图谱的相似度

本文采用t检验法评价中药色谱指纹图谱的相似度。利用来自六个不同厂家的三黄片样品的高效液相色谱指纹图谱数据来验证t检验法的适用性,并用主成分分析(PCA)进一步验证方法的可行性。在PCA的聚类图上,t检验无显著性差异的样品聚为一类,t检验有显著性差异的样品各为一类。结果表明:用t检验法能客观地反映中药样品间的相似性和差异性。     

Compatibility and Stability Studies of Propranolol Hydrochloride Binary Mixtures and Tablets for TG and DSC-photovisual

This study demonstrates the thermalanalysis applications in compatibility and stability studies of the propranolol binary mixture sand tablets A and B. The propranolol binary mixtures were prepared in the laboratory and compared to the fully formulated tablets using the thermogravimetric (TG) and calorimetric(DSC) methods. DSC of binary mixtures showed similar phase transition to propranolol drug. The tablets phase transition decreased and there was no detectable significant interaction in propranolol–lactose mixture and tablets. The DSC-photovisual test revealed an interaction similar to the Maillard reaction. The TG isothermal study showed a difference in the profile between the drug and tablets due excipients quality and problems in manufacture process. The kinetic parameters indicated a lower stability for the tablets than propranolol drug. The thermal techniques thermally differentiated the propranolol preparations demonstrating the importance in the design development of pharmaceuticals solid-dosage form. This revised version was published online in July 2006 with corrections to the Cover Date.     

Triazole derivatives as analytical reagents. Part V. Analytical studies of β-resorcylazomercaptotriazole (METRIAREZ-β) and γ-resorcylazomercaptotriazole (METRIAREZ-γ) acids

METRIAREZ- and -, two new derivatives of 5-mercapto-1,2,4-triazole with - and -resorcylic acids have been synthesized and their physicochemical and chelating properties determined. With metal ions havingp andd electrons they form water-soluble coloured chelates at L M molar ratios of 1 1 with Cu²⁺ and Pb²⁺ ( and ), Hg²⁺ and Zn²⁺ () and Cd²⁺, In³⁺ and Bi³⁺ () and 2 1 with Fe³⁺, Fe²⁺, Co²⁺ and Ni²⁺ ( and ) and Zn²⁺ (). The chelates are non-extractable by organic solvents. The stability constants of these complexes, as well as their spectrophotometric sensitivity and extinction coefficients were determined. Iron and zinc in multivitamin tablets were determined spectrophotometrically using the ligands.     

小儿苯巴比妥分散片在家犬体内药代动力学与生物利用度研究

报道了用高效液相色谱法测定小儿苯巴比妥分散片在家犬体内的药代动力学及生物利用度，为临床科学用药提供了依据。     

Electrochemical determination of muscle relaxant drug tetrazepam in bulk form,pharmaceutical formulation,and human serum

Tetrazepam dissolved in the Britton-Robinson universal buffer of various pH values (2.5–11.5) containing 10 vol. % of ethanol was reduced at the mercury electrode in a single 2-electron irreversible step due to reduction of the 4,5 C=N double bond of the seven-membered ring. Differential pulse polarography (DPP) and adsorptive cathodic stripping voltammetry (AdCSV) techniques (Linear sweep LS, differential pulse DP and square-wave SW modes) for quantification of tetrazepam in bulk form and in myolastan tablets are presented. Moreover, the described linear sweep, differential pulse, and square-wave adsorptive cathodic stripping voltammetry was successfully applied in quantification of tetrazepam in spiked human serum without any prior extraction of the drug. The obtained results showed an increased sensitivity of the described electro-analytical procedures for the quantification of tetrazepam in the following order DPP, DP-AdCSV, LS-AdCSV, and SW-AdCSV, since the observed limits of tetrazepam quantitation by these electroanalytical techniques were 5 × 10⁻⁶ mol L⁻¹, 3 × 10⁻⁷ mol L⁻¹, 1 × 10⁻⁸ mol L⁻¹, and 3 × 10⁻⁹ mol L⁻¹, respectively.     

库仑滴定法测定Vitamin C片及黄瓜、青椒中抗坏血酸的含量

建立了以1.0 mol.L-1碘化钾和1.0 mol.L-1醋酸混合液作为电解液的恒电流库仑滴定法测定抗坏血酸含量的方法。结果表明,方法的回收率在98.3%~100.8%之间,RSD在0.21%~0.56%(n=3)。该法可直接用于V itam in C片及黄瓜、青椒等样品中抗坏血酸含量的测定,方法简便灵敏,结果令人满意。     

Identification and quantitative analysis of the chemical constituents of Gandouling tablets using ultra-high-performance liquid chromatography with quadrupole time-of-flight mass spectrometry

Gandouling tablets are used in a clinical agent for the treatment of hepatocellular degeneration; however, their chemical constituents have not been elucidated. Here, we screened and identified the chemical constituents of Gandouling tablets using ultra-high-performance liquid chromatography (UHPLC)-quadrupole time of flight/mass spectrometry. A method for the quality evaluation of Gandouling tablets was developed by combining the UHPLC fingerprints and the simultaneous quantitative analysis of multiple active ingredients. For fingerprint analysis, 20 shared peaks were identified to assess the similarities among the 10 batches of Gandouling tablets and the similarity was >0.9. The levels of nine representative active ingredients were simultaneously determined to ensure consistency in quality. A total of 99 chemical components were identified, including 18 alkaloids, 20 anthraquinones, 13 flavonoids, 11 phenolic acids, 9 polyphenols, 7 phenanthrenes, 5 sesquiterpenes, 3 curcuminoids, 2 lignans, 2 isoflavones, 2 dianthranones, and 7 other components. The retention times, molecular formulae, and secondary fragmentation information of these compounds were analyzed, and the cleavage pathways and characteristic fragments of some of the representative compounds were elucidated. This systematic analysis used to identify the chemical components of Gandouling tablets lays the foundation for its further quality control and research on their pharmacodynamic substances.     

基于标准制剂控制模式和定量指纹图谱评价复方甘草片的质量一致性

通过建立复方甘草片标准制剂（SP）控制模式和定量高效液相色谱指纹图谱,结合5个质量标志物的精准定量评价了9个厂家共145批复方甘草片质量一致性。首先建立了复方甘草片标准制剂的标准指纹图谱（SP-RFP）,然后以SP-RFP作为评价标准,采用系统指纹定量法对145批复方甘草片进行整体定性和整体定量评价。用双标校正法校正定量指纹图谱的系统误差,结果表明所检样品质量均合格。此外,在统一化色谱条件下测定各原料药和模拟样品,对制剂指纹进行归属相关度和准确度评判,得到原料指纹与制剂指纹的相关性,从而实现智能预测制剂或原料药质量和阻止低劣原料入药。同时用紫外全指纹溶出度法测定5个厂家的复方甘草片的溶出度曲线,用以评价制剂工艺的合理性。以上方法可行且准确度高,实现了对复方甘草片质量和工艺的一致性评价。该文为中药质量一致性评价提供了基础评价模式和基本操作思路以及具体实例。     

4种过期感冒药品的太赫兹光谱研究

针对近期几起过期药品致病的负面消息,为进一步提高药品质量检测的速度,提出采用太赫兹时域光谱技术（THz-TDS）无损检测药品质量的新方法。首先,通过飞秒激光器以及THz-TDS系统（Z-3）检测过期阿莫西林胶囊、复方氨酚烷胺片、板蓝根颗粒和复方板蓝根颗粒等常用感冒药的太赫兹时域光谱。然后,通过快速傅里叶变换（FFT）,得到其太赫兹脉冲随频率变化的频谱图。接着,根据Dorney和Duvillaret等提出的THz-TDS提取光学参数模型,得到以上4种感冒药品的太赫兹特征吸收峰、吸收系数图谱和折射率。最后,将上述实验结果与相关文献报道的太赫兹特征吸收峰、吸收系数以及折射率进行对比。实验显示：过期阿莫西林胶囊和复方氨酚烷胺片在有效频段0.2~0.9 THz内的平均折射率分别为1.90和1.85,这比相关文献分别报道的最小折射率1.92和2.05小;过期板蓝根颗粒和复方板蓝根颗粒在有效频段0.2~1.4 THz内的平均折射率均为1.84,这较相关文献报道的最大折射率1.797略大;过期阿莫西林胶囊的5个太赫兹特征吸收峰均出现,但幅值有所降低;过期复方氨酚烷胺片的3个太赫兹特征吸收峰仍然存在,但幅值也有所降低,且在1.50 THz附近出现新的太赫兹特征吸收峰;过期板蓝根颗粒在1.43 THz出现新的太赫兹强特征吸收峰,且吸收系数减小;过期复方板蓝根颗粒在1.43,1.48和1.54 THz出现3个新的太赫兹特征吸收峰,且吸收系数也减小。结果表明：过期阿莫西林胶囊、复方氨酚烷胺片、板蓝根颗粒和复方板蓝根颗粒的有效成分均有所减少,部分化学成分已经发生改变;过期阿莫西林胶囊和复方氨酚烷胺片等西药的折射率会增大,而过期板蓝根颗粒和复方板蓝根颗粒等中药的折射率会减小;通过折射率的变化和太赫兹特征吸收峰位置的不同以及新出现的太赫兹特征吸收峰,可以区分以上4种过期药品,由此可以为太赫兹光谱技术区分过期药品提供参考。     

近红外光谱法同时快速测定五种抗结核药物的主成分含量

20世纪80年代以来,全球的结核病形势急剧恶化,利福平片、异烟肼片、吡嗪酰胺片、异福片和异福酰胺片是目前比较有效的抗结核药物.文章采用近红外光谱技术(NIRS)结合偏最小二乘法(PLS)建立了同时测定上述五种抗结核药物中的利福平(RMP)、异烟肼(INH)和吡嗪酰胺(PZA)含量的定量分析模型.实验结果表明,采用原始光谱建立模型测定以上抗结核药物中各组分含量时,测定RMP含量的最有效的波长范围为1 981～2 195啪,测定INH含量的最有效波长范围分别是1 540～1 717nm和2 086～2 197 nm,测定PZA含量的最有效波长范围分别是1 460～1 537 nm,1 956～2 022 nm和2 268～2 393 nm,最优模型测定RMP,INH和PZA含量的交互验证均方根误差(RMSECV)分别为0.049 4,0.025 7和0.030 7,模型对预测集样品中的RMP,INH和PZA含量预测,预测均方根误差(RMSEP)分别为0.034 9,0.016 6和0.013 4,预测相关系数(rp)分别达到0.986 4,0.998 9和0.999 3,表明模型预测准确可靠,该研究对抗结核药物生产中质量检验和在线检测有重要的意义.