高效液相色谱法测定五味子和含五味子的制剂中五味子乙素及多种活性成分时流动相体系的选择

建立了用高效液相色谱法测定五味子和含五味子的制剂中五味子乙素的流动相体系。用Shim-pack VP-ODS (250 mm×4.6 mm,5 μm)色谱柱,在柱温30 ℃、检测波长285 nm、流速1.0 mL/min的条件下,用不同的流动相组成及其不同比例研究了五味子提取液中3种木脂素(五味子乙素、安五脂素和五味子甲素)的保留时间及其分离情况,从中选择测定五味子乙素的最佳流动相体系。结果表明,在甲醇-水、甲醇-冰醋酸-水的流动相体系中,安五脂素和五味子乙素很难完全分离;而在乙腈-甲醇-水和乙腈-冰醋酸-水流动相体系中,3种木脂素可很好地分离。以乙腈-甲醇-水(体积比为17:58:25)为流动相测定五味子和护肝片中3种木脂素的含量,相对标准偏差(n4)为0.95%～5.8%,平均加标回收率为94.50%～105.6%。将该流动相体系用于供试品中3种木脂素含量的测定,分离效果好,结果令人满意。     

毛细管气相色谱法测定中药材中多种拟除虫菊酯农药残留量

研究了气相色谱法测定中药材中多种拟除虫菊酯类残留量的分析方法。样品经正己烷．丙酮混合液[V（正己烷）：V（丙酮）=1：1]提取,氟罗里硅土层析柱净化,采用毛细管色谱柱分离,GC-ECD可同时测定8种拟除虫菊酯类农药残留量,回收率为76．6％～104．2％。     

中药材提取物的混批勾兑研究

采用非线性最小二乘拟合计算中药材提取物的勾兑系数,不同批的中药材提取物经过勾兑后与参照样品的差异减小,各成分含量稳定。采用数据预处理的方法,并对数据预处理方法进行改进,使峰面积较小的色谱峰可以实现较小的相对差异。引入误差控制系数,可实现对特定色谱峰的控制要求。实验结果表明,非线性最小二乘拟合可以用于计算中药材提取物的勾兑系数。     

流动注射化学发光法测定中药材中没食子酸

建立快速简便的流动注射化学发光分析法,用于中药材中没食子酸含量的测定.利用酸性介质中Fe3+-H2O2体系生成羟基自由基氧化没食子酸产生微弱的化学发光,用罗丹明6G来增敏化学发光.研究了影响化学发光的各种因素,探讨了可能的机理.结果表明,0.18 mol/L HCl,0.04 mol/L FeCl3,1.0 mol/L H2O2与1.0×10-4 mol/L罗丹明6G溶液组成最优的化学发光体系,没食子酸浓度在1.0×10-5～1.0×10-2 g/L和0.01～1.0 g/L范围内与化学发光强度呈很好的线性关系,r分别为0.9984和0.9947,检出限为3.0×10-6 g/L.对1.0×10-4 g/L没食子酸平行测定11次的相对标准偏差为3.8%.利用本方法成功地测定了中药材诃子和没食子中的没食子酸含量.     

抗病毒类中草药中三种微量元素的测定

采用硝酸和高氯酸(4+1)混合酸消解样品,火焰原子吸收光谱法测定了抗病毒类中草药板蓝根、金银花、鱼腥草中Fe、Cu、Zn 3种微量元素的含量.结果表明,3种抗病毒类中草药中Fe含量相对较高,Zn含量次之,Cu含量相对较低,RSD＜1.60%,回收率在94%～104%之间,方法具有良好的准确度和精确度.     

Herbal medicine analysis by liquid chromatography/time-of-flight mass spectrometry

The fact that the effects of herbal medicines (HMs) are brought about by their chemical constituents has created a critical demand for powerful analytical tools performing the chemical analysis to assure their efficacy, safety and quality. Liquid chromatography coupled to mass spectrometry (LC–MS) is an excellent technique to analyze multi-components in complex herbal matrices. Due to its inherent characteristics of accurate mass measurements and high resolution, time-of-flight (TOF) MS is well-suited to this field, especially for qualitative applications. The purpose of this article is to provide an overview on the potential of TOF, including the hybrid quadrupole- and ion trap-TOF (QTOF and IT-TOF), hyphenated to LC for chemical analysis in HMs or HM-treated biological samples. The peculiarities of LC–(Q/IT)TOF-MS for the analysis of HMs are discussed first, including applied stationary phase, mobile-phase selection, accurate mass measurements, fragmentation and selectivity. The final section is devoted to describing the applicability of LC–(Q/IT)TOF-MS to routine analysis of multi-components, including target and non-target (unknown) compounds, in herbal samples, emphasizing both the advantages and limitations of this approach for qualitative and quantitative purposes. The potential and future trends of fast high-performance liquid chromatography (HPLC) (e.g. rapid resolution LC and ultra-performance LC) coupled to (Q)TOF-MS for chemical analysis of HMs are highlighted.     

Role of counter-current chromatography in the modernisation of Chinese herbal medicines

This review focuses on the growing popularity of using counter-current chromatography (CCC), with its liquid stationary phase, as one of the prime methods for isolating compounds from Chinese herbal medicines (CHMs). 198 publications are reviewed covering 108 different plant species from 56 plant families. These describe the isolation of 354 different molecules across a wide range of polarities, chemical classes and molecular weights (in the range 100–1000 Da). The suitability of CCC for the separation of active compounds from CHM, the phase systems used, how CCC has developed in China, compounds isolated, CCC instrumentation, performance, operational issues and innovations, all supported by detailed cross-referencing, are described. It is concluded that CCC is making an increasingly important contribution to the modernisation of Chinese herbal medicines.     

高效液相色谱-电感耦合等离子体质谱(ICP-MS)法测定中药材中无机汞、甲基汞、乙基汞

为准确测定中药材中不同形态的汞含量,通过选用人工胃液作为提取液,经水浴加热提取后,以甲醇-乙酸铵为流动相,采用C18反相色谱柱对样品溶液进行分离,最后经电感耦合等离子体质谱(ICP-MS)法测定3种汞形态化合物的含量。建立了中药材中无机汞、甲基汞、乙基汞的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)法的测定方法,结果表明,3种汞形态化合物在0.5～5 ng/mL范围内均获得良好的线性关系,相关系数均大于0.999。通过加标回收的方法进行准确性评价,加标回收率为75.5%～118%,相对标准偏差RSD为2.4%～9.7%。测定的106批次中药材中,均未检出甲基汞、乙基汞。无机汞检出率为88.7%,合格率为100%。方法能够准确、高效地测定中药材中3种汞形态化合物的含量。106批次中药材中的汞存在形态主要是以无机汞为主。考察的106批次根及根茎类中药材中3种汞形态化合物的含量,积累了基础数据,为中药饮片的质量安全性监管提供技术支撑。     

Fast Screening of Biomembrane-Permeable Compounds in Herbal Medicines Using Bubble-Generating Magnetic Liposomes Coupled with LC–MS

A novel strategy based on the use of bionic membrane camouflaged magnetic particles and LC–MS was developed to quickly screen the biomembrane-permeable compounds in herbal medicines. The bionic membrane was constructed by bubble-generating magnetic liposomes loaded with NH₄HCO₃ (BMLs). The lipid bilayer structure of the liposomes enabled BMLs to capture biomembrane-permeable compounds from a herbal extract. The BMLs carrying the compounds were then separated from the extract by a magnetic field. Upon heat treatment, NH₄HCO₃ rapidly decomposed to form CO₂ bubbles within the liposomal bilayer, and the captured compounds were released from BMLs and analyzed by LC–MS. Jinlingzi San (JLZS), which contains various natural ingredients, was chosen to assess the feasibility of the proposed method. As a result, nine potential permeable compounds captured by BMLs were identified for the first time. Moreover, an in vivo animal study found that most of the compounds screened out by the proposed method were absorbed into the blood. The study provides a powerful tool for rapid and simultaneous prediction of multiple biomembrane-permeable components.     

The Potential of Parsley Polyphenols and Their Antioxidant Capacity to Help in the Treatment of Depression and Anxiety: An In Vivo Subacute Study

Depression and anxiety are major mental health problems in all parts of the world. These illnesses are associated with a number of risk factors, including oxidative stress. Psychotropic drugs of a chemical nature have demonstrated several side effects that elevated the impact of those illnesses. Faced with this situation, natural products appear to be a promising alternative. The aim of this study was to evaluate the anxiolytic and antidepressant effects of the Petroselinum sativum polyphenols in vivo, as well as its correlated antioxidant properties in vitro. Anxiolytic activity of the extract (50 and 100 mg/kg) was evaluated using the open field and the light-dark chamber tests, while the antidepressant activity was evaluated using the forced swimming test. The antioxidant activity of the extract was evaluated by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical test and the FRAP (iron-reducing capacity) test. The phenolic extract showed very powerful anxiolytic and antidepressant-like effects, especially at a dose of 100 mg/kg, decreasing the depressive behavior in mice (decreased immobility time) and also the anxiolytic behavior (tendency for discovery in the center and illuminated areas) better even than those of paroxetine and bromazepam (classic drugs) concomitant with those results the extract also showed an important antioxidant capacity. These preliminary results suggest that Petroselinum sativum exhibits anxiolytic and antidepressant potential for use as a complement or independent phytomedicine to treat depression and anxiety.