煎煮对几种特色南药中重金属元素含量和形态影响

考察了几种特色南药中重金属(Cd,Cr,Cu,Fe,Mn,Ni,Pb,Sr,Zn)的含量状况,并采用形态连续萃取法分析重金属在药材中的形态分布,研究了药材煎煮时药材中重金属的释放及煎煮过程对药材中重金属形态分布的影响。结果表明,几种南药中Cr,Pb,Zn的含量较高,且巴戟天中的重金属总量高于限量标准;原药材中Cr,Cu,Mn,Ni,Pb和Zn主要存在于有机态和残留态,Fe和Sr主要存在于残留态。煎煮使南药中大量重金属迁移到药汤中;药汤中Cu,Mn,Cr,Pb和Zn主要来自于其在药材中的可交换态、碳酸盐结合态和有机态,而药汤中Sr,Ni和Fe不仅包含其非残留态,更多来自于它们的残留态。为减少药汤中重金属,对于Cu,Mn,Cr,Pb和Zn既要控制在药材中的总量,且需降低它们在药材中的非残留态含量;对于Fe,Ni和Sr则主要是控制其在药材中的总量。     

微波消解-ICP-AES法测定蒙药通拉嘎-5中的多元素

采用微波消解-ICP-AES法测定了蒙药通拉嘎-5中的Fe、Cu、Cd、Ca、Mg、Mn、Zn、Sr、Co、Ni、Cr 11种金属元素的含量。结果表明,微波消解法具有快速、高效、节约试剂的优点,由于样品在高压密封系统中进行消解,避免了污染,过程易于控制,消解效率高。测定方法的回收率为98.0%~105.5%,RSD为0.6%~2.4%。蒙药通拉嘎-5中含多种金属元素,尤其Ca、Mg、Sr、Fe、Zn的含量较高。     

HPLC-ICP-MS测定中药中砷的形态

报道了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术测定中药中砷的形态.采用阴离子交换柱,以含0.2 mmol/L乙二胺四乙酸(EDTA)和2 mmol/L NaH2PO4的水溶液为流动相,pH 6.0,流速为1.0 mL/min,成功分离了亚砷酸(AsⅢ)、砷酸(AsⅤ)、甲基砷(MMA)和二甲基砷(DMA).检出限分别为0.67 μg/L (AsⅢ),0.85 μg/L (DMA),0.43 μg/L (MMA),0.70 μg/L (AsⅤ).中药样品经过(1 1)甲醇水溶液超声提取,离心、过滤、氮气吹干甲醇,超纯水定容.样品加标平均萃取回收率分别为: 92.8% (AsⅢ),108% (DMA),104% (MMA),101% (AsⅤ),RSD (n=7)均小于10%.     

埃博霉素的合成

埃博霉素(Epothilones)是一类新的具有抗癌活性的化合物, 其作用机理与紫杉醇相似。对天然埃博霉素及其衍生物的主要全合成进行了综述.     

藏药"帕朱胶囊"中微量元素及重金属元素分析

为探讨藏药“帕朱胶囊”中微量元素与其治疗胃病的相关性,以及监测藏药中的重金属含量,采用原子吸收分光光度法,对帕朱胶囊中的11种元素进行了测定。结果表明,帕朱胶囊中Fe元素含量较高,并含有Cu、Zn、Mn、Se等与治疗胃病直接相关的微量元素,重金属元素Pb、As、Hg含量不超标。为研究传统藏药帕朱胶囊的药效物质基础和安全使用,提供了科学依据。     

Atomic spectrometry and trends in clinical laboratory medicine

Increasing numbers of clinical laboratories are transitioning away from flame and electrothermal AAS methods to those based on ICP-MS. Still, for many laboratories, the choice of instrumentation is based upon (a) the element(s) to be determined, (b) the matrix/matrices to be analyzed, and (c) the expected concentration(s) of the analytes in the matrix. Most clinical laboratories specialize in measuring Se, Zn, Cu, and Al in serum, and/or Pb, Cd, Hg, As, and Cr in blood and/or urine, while other trace elements (e.g., Pt, Au etc.) are measured for therapeutic purposes. Quantitative measurement of elemental species is becoming more widely accepted for nutritional and/or toxicological screening purposes, and ICP-MS interfaced with separation techniques, such as liquid chromatography or capillary electrophoresis, offers the advantage of on-line species determination coupled with very low detection limits. Polyatomic interferences for some key elements such as Se, As, and Cr require instrumentation equipped with dynamic reaction cell or collision cell technologies, or might even necessitate the use of sector field ICP-MS, to assure accurate results. Nonetheless, whatever analytical method is selected for the task, careful consideration must be given both to specimen collection procedures and to the control of pre-analytical variables. Finally, all methods benefit from access to reliable certified reference materials (CRMs). While a variety of reference materials (RMs) are available for trace element measurements in clinical matrices, not all can be classified as CRMs. The major metrological organizations (e.g., NIST, IRMM, NIES) provide a limited number of clinical CRMs, however, secondary reference materials are readily available from commercial organizations and organizers of external quality assessment schemes.     

Gas chromatography-mass spectrometry following pressurized hot water extraction and solid-phase microextraction for quantification of eucalyptol, camphor, and borneol in Chrysanthemum flowers

Chrysanthemum flower is a common traditional Chinese medicine (TCM). In this work, pressurized hot water extraction (PHWE) followed by headspace solid-phase microextraction (HS-SPME) and GC-MS was developed for the determination of three main active volatile compounds of eucalyptol, camphor, and borneol in Chrysanthemum flowers from four different growing areas in China by internal standard method. The parameters of PHWE and HS-SPME were optimized. The method was also validated. The results showed that PHWE-SPME-GC-MS is a simple, rapid, efficient, and solvent-free technique for the quantitative determination of eucalyptol, camphor, and borneol in TCMs and is potentially useful for the TCM quality assessment.     

中国的中药微量元素研究Ⅱ.微量元素:中药有效药成分的核心组分

在中国开展的中药微量元素研究证明,中药有效药成分由有机药成分和无机药成分组成,两者共生共存。从含水络合离子、天然有机金属配合物、中药有机药成分-微量元素配合物,以及中药有机药成分-微量元素复合物四个方面,论述了微量元素在中药有效药成分中的核心地位和核心作用。     

Evaluation and application of a mixed‐mode chromatographic stationary phase in two‐dimensional liquid chromatography for the separation of traditional Chinese medicine

In this study, two mixed‐mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two‐dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed‐mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed‐mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off‐line 2D‐LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine—Uncaria rhynchophylla. The two‐dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed‐mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications.