基于ICP-MS分析的苜蓿矿质元素含量特征与评价

为了探明进口和国产苜蓿总体矿质差异,以国产和进口苜蓿为对象,采用石墨消解-电感耦合等离子体质谱(IC P-M S)法分析干草中磷、钾和锌等17种矿质元素的含量特征,并对矿质元素含量进行了相关性、主成分分析和评价.结果表明,苜蓿干草中矿质元素种类丰富而含量变异较大,平均含量最高的是K元素,其次是Ca>M g>Na>P,A...     

墨龙系列酒中无机元素含量研究

采用荧光、原子荧光、火焰光度、电感耦合等离子发射光谱法测定了墨龙醇、弥猴桃乳酒、麒麟玉液中的27种无机元素。其中钾、镁、磷、钠、钙和铁、锰、锌、铜、锶、镍、铬等人体必需宏、微量元素含量丰富，含量和分别占所测元素加和量的99．0％～99．8％；而有害微量元素铅、汞、镉、铍含量较低，仅占0．005%～0.009%，远低于致毒量。     

金花茶花朵中微量元素的研究

对金花茶花朵不同部位微量元素的含量进行了分析研究.采用微波消解样品,电感耦合等离子体原子发射光谱法同时测定钾、钠、钙、镁、磷、铜、铁、锌、锰、钼、镍、铅、镉、铬的含量.结果表明,花朵中富含微量元素,且而各元素含量在花瓣、花蕊、花粉之中差异较大,为进一步开发金花茶的花朵提供依据.     

新生儿脐血清微量元素测定及与生长发育关系研究

应用电感耦合等离子体发射光谱法测定也３３名新生儿脐血清中１７种微量元素（铁、铜、锰、锌、钴、钼、硒、铬、锡、钒、硅、镍、镉、铅、锶、钛、铝）及３种常量元素（钙、磷、镁）的含量。结果表明,新生儿脐血清微量元素性别分布接近,仅女婴血清铬、钒高于男婴,但地区差异明显,城镇新生儿脐血清中锰、锌、锶、钛、钙较高,而钼、硒、铬、铝较低。多元回归分析显示,血清元素铁、锰、锌、硒、硅、锶、钙被引人新生儿体重和发育     

电感耦合等离子体原子发射光谱法测定8种蔬菜中微量元素

将电感耦合等离子体原子发射光谱法(ICP-AES)应用于 8 种蔬菜中钙、铝、铜、铁、锰、锌、铬、汞、磷、硒、镁、砷、镉、铅、钾、钠等16种微量元素的测定.方法中给出了仪器的工作条件,并叙述了分析谱线的选择,采用微波加热方法对试样进行消解.16 种微量元素的检出限在 0.3～30.0 μg·L-1之间,经试验得出各元素的回收率在 94.3%～104.8%之间.     

茶叶中多种元素的ICP-AES测定

利用电感耦合等离子体发射光谱法(ICP—AES),同时测定了茶叶中的磷、锰、钙、镁、铝、铁、钾、锌、钴、镍、铅、铜、钒、锶的含量。采用元素间干扰系数法校正元素之间的光谱干扰。回收率在86％～108％,RSD为0.6％～9.5％,结果令人满意。     

ICP-MS法测定欧盟玩具新指令限制的17种可迁移元素

根据欧盟玩具安全新指令( 2009/48/EC)的要求,应用电感耦合等离子体质谱(ICP-MS)法测定玩具材料中硼、铝、铬、锰、钴、镍、铜、锌、砷、硒、锶、镉、锡、锑、钡、汞、铅17种可迁移元素含量,使用碰撞反应池技术消除某些多原子离子干扰.方法检出限为0.5～75μg/kg,加标回收率在85.4％～109％之间,相对...     

急性脑血管病患者血清元素的测定

采用高频等离子体发射光谱法测定了３４例脑梗塞、３３例脑出血和对照组２７人血清锌、铜、锰、铬、镁、钼、锶、铁、钛、钡、镉和钙共１２种元素的含量。结果显示脑梗塞和脑出血组血清锌和锌／铜比值显著高于对照组；锰和钼含量仅在脑梗塞组明显增高，锶仅在脑出血组显著增高，而其它几种元素疾病组与对照组无显著性差异。伴有高血糖、高血脂和高血压的病人，其血铬含量显著降低，表明锌、锌／铜比值、锰、钼、锶、铬元素与急性脑血     

基于ICP-MS分析的苜蓿矿质元素含量特征与评价

为了探明进口和国产苜蓿总体矿质差异,以国产和进口苜蓿为对象,采用石墨消解-电感耦合等离子体质谱(ICP-MS)法分析干草中磷、钾和锌等17种矿质元素的含量特征,并对矿质元素含量进行了相关性、主成分分析和评价。结果表明,苜蓿干草中矿质元素种类丰富而含量变异较大,平均含量最高的是K元素,其次是Ca>Mg>Na>P,Al元素含量显著高于其他11种微量元素。Cu、K、Mg、Al、K、Ca两两元素间存在极显著正相关(p<0.01);Ca、Cu、Mg、K、Zn、Co和Na是苜蓿干草的主要特征矿质元素,累积方差贡献率达74.90%。进口苜蓿中K、Ca、Mg、Cu含量显著高于国产苜蓿,而国产苜蓿中Na和Co含量显著高于进口苜蓿。针对国产苜蓿营养缺乏,应在选种和肥料管理中重视增施钾肥和其他微量元素,合理利用苜蓿草产品。     

电感耦合等离子体发射光谱(ICP-OES)法测定泡菜在腌渍过程中矿物质元素的含量变化

按四川传统方式制作泡菜,用硝酸-过氧化氢作消解剂,微波消解预处理样品,电感耦合等离子体发射光谱(ICP-OES)法测定泡菜制作过程中样品的钾、钠、钙、镁、锌、铁、铜、硒、镉、铅、铬等12种矿物质元素的含量变化。结果表明,在乳酸自然发酵环境下,蔬菜腌渍的前5d,除钠外,所测6种样品中钙、镁、锌、铁、铜等11种矿物质元素含量均大幅度降低,致使泡菜软化;且组织结构相近的不同种蔬菜经过较长时间腌制后,各矿物质元素含量基本一致。     

微量热法研究黄连及其主要组分配伍的抑菌作用

基于微量热法,研究黄连、黄连的主要组分小檗碱、药根碱、巴马汀及其配伍模拟方的抑菌作用.以HPLC法测定黄连中小檗碱、药根碱和巴马汀的含量,并根据其含量比值配伍模拟方;微量热法测定黄连、小檗碱、药根碱、巴马汀及其模拟方对痢疾杆菌的生长代谢曲线,得出相应的热动力学参数,并进行对应分析.结果表明黄连、小檗碱、药根碱、巴马汀及其模拟方对痢疾杆菌的生长代谢均有不同程度的抑制作用,黄连作用最强,单体生物碱作用弱,配伍模拟方作用增强,但并未显现明显协同作用,黄连的抑菌作用可能为多种活性成分的综合作用.     

多金属结核/结壳中稀土元素的富集特征及其资源效应

多金属结核/结壳是海洋中最重要的固体沉积矿产之一,蕴藏丰富的铁、锰、铜、钴、镍等金属元素,也是稀土元素的富集体.利用等离子质谱仪/光谱仪对太平洋、大西洋、印度洋及南海北部海多金属结核/结壳11个样品25份试样的稀土含量进行了分析,多金属结核/结壳中稀土平均含量为1265 57×10-6,其中结核平均含量为1096.96×10-6,结壳平均含量1623.88×10-6,人人超过地壳和玑积岩的平均含量.稀土元素的富集主要受控于结核/结壳中铁、锰氧化物及粘土矿物对海水和沉积物中稀土元素的吸附作用,Ce元素高度富集,使其成为多金属结核/结壳矿产开发中可能最先利用的稀土元素之一.     

Determination of Coptis Chinensis Franch and Phellodendron Amurense Rupr in Qingwei-Huanglian Wan by Pls-HPLC Method

Abstract

Coptis chinensis Franch contains berberine(1), palmatine(2), jatrorrhizine(3) and etc. And phellodendron amurense Rupr also contains above components. Qingwei-Huanglian Wan is made from Coptis chinensis Franch, phellodendron amurense Rupr and etc. Berberine, palmatine and jatrorrhizine in Qingwei-Huanglian Wan were determined by HPLC. The optimal composition of mobile phase CH₃COOEt-HCOOH-EtOH (15:3:2) for HPLC separation of berberine, palmatine and jatrorrhizine was successfully determine by using window diagram technique. Detection wavelength was 345nm. Flow rate: 1.5ml/min. Calibration graphs for (1), (2) and (3) were rectilinear for 0.06–0.39μg, 0.06–0.61μg and 0.01–0.12μg respectively. The basic principle and method of partial least squares method (PLS) is presented in this paper. The data from HPLC were treated with PLS program to obtain the contents of Coptis chinensis corresponding with the requirement. All these indicate that PLS-HPLC method is new and feasible for the determination of crude drugs in Chinese Patent Medicine.

2. PLS is a new multivariate statistical method, and its performance is better than other traditional methods such as ordinary multivariate regression and principal components regression. This is because the calibration technique, which makes good use of the information in concentration matrix Y and content matrix X, is used in PLS method.

3. The method is applicable to the quanlity control of the products. The contents of IV and V in VI can be predicted accurately fast, if the method described here is used by factories making VI.     

野生与施肥种植川西獐牙菜中矿物质元素含量的季节变化

为对比野生与施肥（尿素和磷酸二铵）种植青海川西獐牙菜中元素含量的变化,分别采集野生和6～10月施肥种植川西獐牙菜全植株,采用原子吸收光谱仪分析测定了其钾、钠、钙、镁等矿物质元素含量和铜、锌、铁、锰、钴等微量元素含量。结果表明,施肥种植川西獐牙菜中矿物质元素、微量元素含量除钾外,均高于野生种,并在9～10月份达到最高水平,可替代野生种人药,按需适时采收,以解决资源匮乏。     

Affinity chromatography with immobilized DNA stationary phase for biological fingerprinting analysis of traditional Chinese medicines

A stationary phase for high performance affinity chromatography with immobilization of DNA onto silica gel was prepared and characterized. The effect of the ionic strength, concentration of Mg2+, EDTA and CH3CN in the mobile phase on the retention of alkaloids were investigated. With this stationary phase, biological fingerprinting analysis of traditional Chinese medicines (TCMs) Coptis chinensis Franch and Rheum palmatum L. was performed with both one-dimensional (1-D) and two-dimensional (2-D) chromatography. The 1-D chromatography was performed with isocratic and gradient elution and 2-D chromatography was developed with immobilized DNA column combined with silica monolithic ODS column. It was found that 7 compounds in Coptis chinensis Franch including berberine, palmatine and jatrorrhizine, 14 compounds in Rheum palmatum L. including aloe-emodin, rhein, emodin, chrysophannol-8-O-glucophranoside and physionl-8-O-glucophranoside were active in binding to the immobilized DNA.     

野生与种植青海川西獐牙菜中矿物质元素含量特征

青海地道中藏药材川西獐牙菜人工种植试验初见成效。为了对比野生与种植青海川西獐牙菜中矿物质元素的变化,分别采集野生与种植青海川西獐牙菜种子采收前后的全植株,采用原子吸收光谱仪分析测定了其钾、钠、钙、镁等矿物质元素含量。结果表明,野生川西獐牙菜中,青海玉树较四川川西地区的钠、磷元素含量高,钙、钾、镁元素含量低。种植青海川西獐牙菜在成熟种子采收后较采收前钠、镁、钙、磷等显著增加,且种植青海川西獐牙菜与青海玉树地区野生川西獐牙菜中矿物质元素含量较为接近。     

X-射线荧光光谱测定甜瓜中矿质元素

报道了日本理学3080E3型X-射线荧光光谱仪在测定甜瓜样品常量和微量矿质元素中的应用。以国家植物标准参考物质(GBW)为校准标样,采用真空加热干燥法制备甜瓜样品,所得分析结果与ICP-AES对照相吻合。     

Biological fingerprinting analysis by liquid chromatography/mass spectrometry for evaluation of DNA structural selectivity of multiple compounds in natural products

A method by combination of centrifugal ultrafiltration (CUF) sampling with liquid chromatography-mass spectrometry (LC-MS) analysis was established to evaluate the DNA structure and sequence selectivity of the multiple compounds in a small molecule library. The developed method was applied to analyze the extracts of natural products Coptis chinensis Franch and Rheum palmatum (L.). From the obtained biological fingerprinting chromatograms, 7 compounds in C. chinensis Franch and 11 in R. palmatum (L.) were screened out as DNA binding agents. Most of these compounds were identified by standards and LC-MS analysis after the sample pretreatment with the DNA immobilized cartridge. DNA structural binding preference of the multiple active compounds in these two extracts was then evaluated simultaneously without purification.     

Headspace solid-phase microextraction combined with GC×GC-TOFMS for the analysis of volatile compounds of Coptis species rhizomes

In this study, the investigation of the volatile compounds of dried rhizomes of Coptis chinensis Franch, C. deltoidea C. Y. Cheng et Hsiao, and C. teeta Wall was carried out to complete the chemical composition of these valuable natural products. Volatile profiles were established and compared after headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm) fibre coupled to comprehensive 2D gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS). Analyses were performed and compared on two column-phase combinations (non-polar/polar and polar/non-polar). The majority of the identified compounds eluted as well-separated (pure) components as a result of high-resolution capability of the GC×GC method, which significantly reduces co-elution. Therefore, this increases the likelihood that pure mass spectra can be obtained. More than 290 volatile and semi-volatile organic compounds were tentatively characterized by means of GC×GC in tandem with TOFMS detection. Improved result interpretations were obtained in terms of compound classification based on the organized structure of the peaks of structurally related compounds in the GC×GC contour plot. These compounds are distributed over the chemical groups of hydrocarbons, acids, alkenes, alkynes, aldehydes, ketones, alcohols, esters, furans, and terpenoids. Among all the chemical groups, terpenoids present the higher number of identified compounds (44), alkenes (41), and aldehydes and ketones (28). This study completed the volatile phytochemical analysis of the headspace composition of various Coptis species rhizomes, and should serve as a means to identify the difference between the rhizomes and may also be useful to confirm individual species based on their volatile chemical profile.     

Absorption and translocation of nitrogen in rhizomes of Leymus chinensis

Leymus chinensis is a dominant species in the Inner Mongolia steppe, northern China. Plant growth in northern China grassland is often limited by low soil nitrogen availability. The objective of this study is to investigate whether rhizomes of Leymus chinensis are involved in the contribution of N uptake. The N concentration, ¹⁵N concentration and ¹⁵N proportion in roots, rhizomes and shoots after 48 h exposure of roots (L_root) and rhizomes (L_rhizo) separately and roots and rhizomes together (L_r+r) to 0.1 mM ¹⁵NHNO₃ solution were measured using root‐splitting equipment and stable isotope (¹⁵N) techniques, respectively. The N content and dry mass were not affected by the labeling treatment. In contrast, the ¹⁵N concentration in shoots, rhizomes and roots was significantly increased by the labeling in rhizomes, indicating that the inorganic nitrogen was absorbed via rhizomes from the solution and can be transported to other tissues, with preference to shoots rather than roots. Meanwhile, the absolute N absorption and translocation among compartments were also calculated. The N absorption via rhizomes was much smaller than via roots; however, the uptake efficiency per surface unit via rhizomes was greater than via roots. The capacity and high efficiency to absorb N nutrient via rhizomes enable plants to use transient nutrient supplies in the top soil surface. Copyright © 2011 John Wiley & Sons, Ltd.