补益中药材中重金属和残留农药的净化技术研究

The cultivation of Chinese herbal medicine (CHM) requires the use of pesticides to reduce pest damage. Improper use of pesticides not only pollutes the cultivating soil, and ground water, but also leads to accumulation of pesticides in the plants. The risk to health due to the incidental intake of contaminants in CHM by the consumers is highly possible. The organochlorine pesticides (OCPs) are the first target residual contaminants because they possess a long half-life, high accumulation, potential, harmful biological effects, and detrimental impacts on the environment. The need to depuration residual contaminants in CHM becomes apparent. In the study, the supercritical fluid extraction was developed to depuration of heavy metals and the OCPs residue in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng.(1)Development of a supercritical fluid extraction method for the depuration of heavy metals and the organochlorine pesticides residue in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng Supercritical fluid extraction (SFE) has shown to be an efficient and rapid method for the isolation of active constituents from crude drugs. The objective of the present study was to investigation the use of an SFE method for receiving high decontamination rate of heavy metals and 12 OCPs residuals in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng and low loss of related composition.(2)Establishment of a capillary gas chromatography method for the determination of the organochlorine pesticides residue in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng A capillary gas chromatography with electron capture detector (CGC-ECD) was established to determine 12 OCPs residue in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng. The samples were extracted by FDA method. The capillary column was DB-1(30m×0.25mm ×0.25μm). The injector temperature and the detector temperature was set at 250℃ and 280℃, respectively. The experiments were carried on the column temperature program as followed: initial temperature was 150℃, rate of 15℃omin-1 to 180℃ (hold 1min), rate of 10℃omin-1 to 210℃ (hold 2min), rate of 15℃omin-1 to 240℃ (hold 10min). The pesticide residues were calculated by external standard method. The method is easy in operation and has good separation and repeatability.(3)Development of heavy metals in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng Atomic absorption spectrophotography (AAS), atomic fluorescence spectrophotography and colorimetry were developed to determine heavy elements (such as Pb, Cd, As, Hg, Sn) in six benefit traditional Chinese medicines. The linenar ranges were 0.00～20.00ppb. The relative standard deviation was less than 0.51% and the recovery was 91%～108%. This method is simple,　rapid and has been applied to the determination of Pb, Cd, As, Hg and Sn with satisfactory results.(4)Development of the reversed-phase HPLC methods for the determination of the active constituents in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng The reversed-phase HPLC methods were developed to determine of the active constituents in Radix Codoposis, Astragali, Herba Epimedii, Angelica sinensis, Rehmanniae Preparate, and Ginseng. The determination of atractylenoide Ⅲ in Radix Codonopsis was carried on an ODS column and the mobile phase consisted of methanol-water (60︰40,V/V). The detector was operated at 220 nm. The calibration curves were linear in the range of 0.5～10.0 μg/ml and correlation coefficient was 0.9994. The recovery (%) was 82.1、85.4 and 88.4, respectively. The RSD was 2.9、1.3 and 2.7, respectively. The determination of Astragaloside Ⅳ in Astragali was carried on an ODS column and the mobile phase consisted of acetonitrile-water (30︰70,V/V). The detector was

中药材中重金属和残留农药已引起国内外的高度重视，迫切需要研究和解决。本研究以党参等无味补益类中药材为例，对其饮片和其煎液应用超临界CO2流体技术和柱色谱技术进行净化处理，经净化处理后，药材饮片和其煎液中重金属和残留农药低于FDA允许标准，而用于评价中药材质量的一组特征组分无显著变化。本研究为中药材的规范化研究奠定基础。..