Advances in Chemical Composition,Extraction Techniques,Analytical Methods,and Biological Activity of Astragali Radix

Astragali Radix (AR) is one of the well-known traditional Chinese medicines with a long history of medical use and a wide range of clinical applications. AR contains a variety of chemical constituents which can be classified into the following categories: polysaccharides, saponins, flavonoids, amino acids, and trace elements. There are several techniques to extract these constituents, of which microwave-assisted, enzymatic, aqueous, ultrasonic and reflux extraction are the most used. Several methods such as spectroscopy, capillary electrophoresis and various chromatographic methods have been developed to identify and analyze AR. Meanwhile, this paper also summarizes the biological activities of AR, such as anti-inflammatory, antioxidant, antitumor and antiviral activities. It is expected to provide theoretical support for the better development and utilization of AR.     

Capillary electrophoresis determination of six bioactive constituents in San-huang-hsieh-hsin-tang

A capillary electrophoretic method for simultaneous determination of six bioactive ingredients (berberine, palmatine, baicalin, sennoside B, emodin, and sennoside A) in the Chinse herbal formula San-huang-hsieh-hsin-tang was established. A carrier composed of aqueous buffer solution (50 mM sodium cholate, 15 mM sodium dihydrogen phosphate, and 4.25 mM sodium borate)-acetonitrile (3:2) was found to be the most suitable electrolyte for this separation. Contents of these constituents in a non-pretreated methanol-water extract of San-huang-hsieh-hsin-tang sample could be easily determined within 20 min. The effects of borate, cholate, and organic modifier (acetonitrile) concentration of the carrier on the migration behavior of the solutes were also studied.     

桔梗等中药微量元素初探

对中药桔梗、怀牛膝,华山参、鹿角胶,龟甲胶及阿胶进行了微量元素研究。结果发现：同一种中药因产地不同,其微量元素的含量不同。同一种植物药,其部位不同,所含微量元素多少不等。同一类型的中药,其品种、来源不同,微量元素的含量高低也不相同。本研究为今后对这些中药进行真伪鉴别,合理开发或综合利用都提供了科学的依据。     

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。     

固相萃取-定量核磁共振波谱法测定板蓝根饮片中的表告依春

建立了固相萃取(SPE)-定量核磁共振波谱(qNMR)技术测定板蓝根饮片中有效成分表告依春含量的方法.样品用水超声提取两次,采用SPE对提取液进行富集浓缩,用qNMR测定表告依春的含量.考察了样品预处理和qNMR实验条件对测定结果的影响,选择氘代二甲基亚砜为溶剂,用基准试剂邻苯二甲酸氢钾标定的2,3,5-三碘苯甲酸为内标,选择脉冲宽度P1=14.1 μs,延迟时间d1=5 s,扫描次数NS=256为qNMR定量测定表告依春的最佳实验条件.表告依春的定量峰为δ 5.365~5.399 (H-7b, d,1H).结果表明,日内测量精密度(RSD)为0.5%,日间精密度为0.8%,表告依春与三碘苯甲酸峰面积比与质量比的零截距标准曲线线性相关系数为0.9991,且斜率与理论值相符.根据响应值标准偏差和标准曲线斜率法确定此法测定表告依春的检测限(LOD)为0.05 mg/g;定量限(LOQ, S/N ≥ 150)为0.19 mg/g.包括样品提取过程的表告依春的回收率为97.4%~101.7%.采用本方法测定板蓝根饮片中的表告依春的含量为<0.19~1.26 mg/g.研究结果表明,采用SPE进行富集,扩大了qNMR的应用范围,可用于低含量复杂样品的定量分析.     

山麦冬、麦冬对照药材电喷雾-质谱(ESI-MS)特征图谱的比较研究

报道了采用电喷雾-质谱负离子全扫描法,分析山麦冬、麦冬对照药材的甲醇提取物。经分析发现,山麦冬、麦冬对照药材负离子的全扫描质谱图差异显著,从中选择16强峰建立山麦冬、麦冬对照药材甲醇提取物的特征图谱。研究表明,该分析方法有较好的重现性,图谱特征性强,可快速、准确鉴别山麦冬、麦冬药材。     

反相高效液相色谱法测定大黄药材中游离及结合型蒽醌类衍生物的含量

建立了同时测定大黄药材中蒽醌类衍生物含量的RP HPLC法。色谱柱为HypersilC1 8柱 (2 5 0mm×4 6mmi.d .,1 0 μm) ,流动相为甲醇 乙腈 水 (3∶5∶2 ,磷酸调pH 2 .8) ,流速为 1 .0mL min ,柱温为 2 5℃ ,检测波长为 2 2 5nm。在此色谱条件下 ,各组分在 2 0min内均得到良好分离。平均回收率为 98.83 %～ 1 0 0 .9% ;相对标准偏差 0 .68%～ 1 .5 8%。     

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%.     

Enhancement by Glycyrrhizae Radix of hepatic metabolism of hypaconitine,a major bioactive and toxic component of Aconiti Laterlis Radix,evaluated by HPLC‐TQ‐MS/MS analysis

Glycyrrhizae Radix (GR) is often prescribed together with Aconiti Laterlis Radix (ALR) (a so‐called compatible drug pair) in traditional Chinese medicinal practice to reduce toxicity of ALR. However, the mechanisms involved remain to be addressed. In this study, the metabolic interactions between GR–ALR drug pair were investigated for the first time. First, an HPLC‐TQ‐MS/MS method was developed to analyze hypaconitine, a major bioactive and toxic component of ALR, in rat liver S9. Then the in vitro metabolic rates of hypaconitine by different rat liver S9 were compared using the established method. The experiments were designed in four groups: pure hypaconitine (group I) and ALR extract (group II) incubated with liver S9 of normal rats, and pure hypaconitine (group III) and ALR extract (group IV) incubated with liver S9 of GR‐pretreated rats. When incubated for more than 4 h, the metabolic rates of hypaconitine in group III were significantly higher than those in group I, and when incubated for more than 2 h, the metabolic rates of hypaconitine in group IV were significantly higher than those in group II, suggesting that GR can enhance metabolic rate of hypaconitine, the mechanism of which might be related to hepatic metabolizing enzyme induction by GR. Copyright © 2012 John Wiley & Sons, Ltd.     

Rapid determination of yunaconitine and related alkaloids in aconites and aconite‐containing drugs by ultra high‐performance liquid chromatography–tandem mass spectrometry

Yunaconitine (YAC) is a toxic aconite alkaloid that is considered to be a hidden aconite poison since it is frequently found in body fluids from aconite poisoning patients, but has not been well studied in commonly used herbal drugs. In this paper, a rapid and sensitive ultra high‐performance liquid chromatography–tandem mass spectrometry (UHPLC‐MS/MS) detection combined with microwave‐assisted extraction (MAE) was developed for high throughput simultaneous determination of YAC and six other toxic aconite alkaloids in 31 samples of crude, processed aconites and aconite‐containing drugs. The optimized method showed excellent linearity, precision, accuracy and recovery for all target compounds with short run time. YAC was detected in some samples with contents from 0.015 to 10.41 mg/g. This is the first report on the determination of YAC in Radix Aconiti, Radix Aconiti Kusnezoffii and aconite‐containing drugs. This newly developed method facilitates the rapid screening of YAC and related toxic aconite alkaloids and allows YAC to be used as a chemical marker for the quality control of aconites and aconite‐containing drugs. Copyright © 2012 John Wiley & Sons, Ltd.