加速溶剂萃取-气相色谱质谱法测定太子参中酰胺类除草剂的含量

建立了太子参中乙草胺、丁草胺和S-异丙甲草胺的加速溶剂萃取-气相色谱/质谱测定的分析方法。对提取溶剂、萃取温度、净化材料、不同冲洗体积和静态萃取时间、循环次数等实验条件进行了优化。用HP-5MS弹性石英毛细管柱经柱程序升温技术分离,并用质谱检测器检测,内标法计算含量。本方法测定太子参中乙草胺、丁草胺和S-异丙甲草胺的检出限分别为0.16 ng/g、0.18 ng/g和0.05 ng/g,精密度分别为2.6%、3.9%和3.1%,回收率为80.2%-104.1%。所测样品不含上述3种除草剂残留。本方法简便、干扰小、检测效果好,可用于太子参药材中此类除草剂残留的分析。     

保证多指标成分含量稳定的中药材最优化调配方法

提出了一种利用HPLC指纹图谱测定中药材多指标成分含量, 再运用线性、非线性最优化理论调配中药材, 从而保证中药材调配物多指标成分含量稳定的新方法. 方法的核心是所提出的7种最优化调配目标函数及相应的约束条件. 实验验证, 以10批板蓝根药材为基础, 在7种最优化目标下, 控制5个主要HPLC色谱峰面积稳定均一, 结果显示, 峰面积最大相对偏差的绝对值为6.3%.     

Authentication of Shenqi Fuzheng Injection via UPLC-Coupled Ion Mobility—Mass Spectrometry and Chemometrics with Kendrick Mass Defect Filter Data Mining

Nearly 5% of the Shenqi Fuzheng Injection’s dry weight comes from the secondary metabolites of Radix codonopsis and Radix astragali. However, the chemical composition of these metabolites is still vague, which hinders the authentication of Shenqi Fuzheng Injection (SFI). Ultra-high performance liquid chromatography with a charged aerosol detector was used to achieve the profiling of these secondary metabolites in SFI in a single chromatogram. The chemical information in the chromatographic profile was characterized by ion mobility and high-resolution mass spectrometry. Polygonal mass defect filtering (PMDF) combined with Kendrick mass defect filtering (KMDF) was performed to screen potential secondary metabolites. A total of 223 secondary metabolites were characterized from the SFI fingerprints, including 58 flavonoids, 71 saponins, 50 alkaloids, 30 polyene and polycynes, and 14 other compounds. Among them, 106 components, mainly flavonoids and saponins, are contributed by Radix astragali, while 54 components, mainly alkaloids and polyene and polycynes, are contributed by Radix codonopsis, with 33 components coming from both herbs. There were 64 components characterized using the KMDF method, which increased the number of characterized components in SFI by 28.70%. This study provides a solid foundation for the authentification of SFIs and the analysis of its chemical composition.     

微波消解ICP-AES法测定不同生长年限白芍的微量元素

采用微波消解技术-电感耦合等离子-原子发射光谱法(ICP-AES)对不同产地、不同生长年限的芍药及其炮制前后含有的几种具有重要生理功能的无机微量元素——K,Ca,Na,Mg,Za,Fe和Cu等的含量进行了依次测定。结果显示样品中含有丰富的微量元素,该方法的RSD均在4%以下,加标回收率在99%～113%,具有较好的准确度和精密度。进而采用主成分分析法(PCA)对所测得的白芍样品微量元素作为变量进行分类研究。结果表明微波消解-电感耦合等离子-原子发射光谱法可同时测定多种微量元素,主成分分析法是不同白芍的分析分类的有效方法,实验结果可为白芍中微量元素与其药效的相关性提供科学依据。     

Characterization of the constituents in rat plasma after oral administration of radix polygoni multiflori extracts by ultra‐performance liquid chromatography/quadrupole time‐of‐flight mass spectrometry

An ultra‐performance liquid chromatography/quadrupole time‐of‐flight mass spectrometry method was established to detect as many constituents in rat plasma as possible after oral administration of Radix polygoni multiflori (RPM) extract. A C₁₈ column (150 × 2.0 mm, 4 µm) was adopted to separate the samples, and mass spectra were acquired in negative modes. The fingerprints of RPM extract were established, resulting in 39 components being detected. Among these compounds, 29 were identified by comparing the retention times and mass spectral data with those of reference standards and relevant references, and eight compounds were separated and detected in RPM for the first time. In vivo, 23 compounds were observed in dosed rat plasma, 16 of 23 compounds were indicated as prototype components of RPM, and seven compounds were predicted to be metabolites of RPM. A high‐speed and sensitive method was developed and was successfully utilized for screening and characterizing the ingredients and metabolites of RPM. Copyright © 2015 John Wiley & Sons, Ltd.     

草乌的拉曼光谱分析

草乌是一种重要的药用和有毒植物之一，本文采用FT-Raman光谱法定性分析了生，熟草乌的组成，结果显示，草乌因加工（熟草乌）和未加工（生草乌）其拉曼光谱有不同，造成这一现象的原因可甬由于生草乌加工泡制成熟草乌所致，即导致熟草乌的毒性低于生草乌，这将有助于生、熟草乌的质量控制与毒性分析。     

苦黄注射液中大黄蒽醌含量测定方法改进

按苦黄注射液原质量标准（草案）中测定方法,大黄蒽醌用氯仿提取,阴性试验结果为苦黄注射液大黄蒽酯标示量的１６．５０％（ｎ＝５）,结果偏高;改用石油醚提取,降为６．１５％,重复性试验的ＲＳＤ为１．４４％（ｎ＝５）,加标回收率为１０１．８％（ｎ＝５）,显色在１－４ｈ内稳定,表明该法是可行的。     

豫产桔梗的土壤与药材中部分微量元素含量与分析

为了解桔梗中微量元素含量特征,研究土壤中微量元素对桔梗药材道地性的影响,采用原子吸收光谱法、冷原子荧光法、双道原子荧光法对不同产地的桔梗药材及生境土壤中8种微量元素含量进行了测定,所得数据用SPSS 11.0软件进行分析比较。结果表明,不同产地的桔梗微量元素含量有差异;药材与土壤中微量元素之间具有相关性。桔梗对土壤中微量元素是主动与被动相结合的有选择吸收。     

中药黄芩中总氮和总磷的测定

采用可见－紫外分光光度法测定了黄芩中总氮和总磷的含量。本法简便，结果准确。