两种降血糖药的元素含量测定及其临床意义

用原子吸收分光光度法测定了两种降解药物中元素含量。结果显示，两种降糖药物中Ｍｎ，Ｚｎ，Ｎｉ较为丰富，明显高于正常值，其中Ｍｎ，Ｆｅ，Ｚｎ高于正常值的２￣１７０倍，提示两种降糖药物的元素含量，对纠正糖尿病含量的元素紊乱，有一定的临床意义，为糖尿病患者选择治疗药物提供了科学的依据。     

垃圾焚烧飞灰颗粒的微观形态特征及能谱研究

利用SEM/EDX，观察了垃圾焚烧飞灰颗粒的微观形态特征，探讨了其主要组成元素及其质量分数。实验结果表明，飞灰颗粒形态多样化，其中以不规则形状聚合体居多，球形体、絮状集合体相对较少，少数颗粒为棒状集合体。球形飞灰颗粒很少有重金属分布，不规则形状聚合体或絮状集合体的表面易分布重金属。从飞灰颗粒表面、内部组成元素的质量分数来看，Si、Ca、Al为主要元素。飞灰颗粒表面、内部有重金属Pb、Cu等分布，局部测定点其质量分数可高达16.2%和14.5%。     

不同批次复方木鸡颗粒中无机元素的差异分析

目的通过测定8批复方木鸡颗粒中无机元素的含量,拟从无机成分的角度探讨复方木鸡颗粒的特征元素。方法采用电感耦合等离子体质谱仪(ICP-MS),以半定量分析的方式测定8批次复方木鸡颗粒无机元素的含量,建立复方木鸡颗粒无机轮廓谱,并对其差异元素中的重金属元素和人体有益元素进行全定量测定,同时,采用聚类分析和主成分分析,对其特征元素进行评价。结果构建了复方木鸡颗粒无机元素的轮廓谱,通过聚类分析和主成分分析共找到6个特征元素,包括Ca、Mg、Mn、K、Cr、Ni。结论从无机成分的角度明确了复方木颗粒的特征元素,为进一步探究复方木鸡颗粒的药效研究提供理论依据。     

大气中单个硝酸盐和硫酸盐颗粒的测定方法

介绍一种测定大气中单个硝酸盐和硫酸盐颗粒的方法，在采用复合薄膜法确定了单个硝酸盐和硫酸盐颗粒的基础上，再利用X射线能谱仪对它们进行元素分析，其中，颗粒中所含的硝酸根离子和硫酸根离子分别由反应生成的针状结晶物和圆环状结晶物来确定，而对应的阳离子则由X射线能谱仪检出，在实验室中对12种大气中常见的硝酸盐和硫酸盐人工颗粒和实际大气颗粒物进行了观察，结果表明该法是可行的。     

高效液相色谱法快速测定参芪降糖胶囊中人参皂苷的含量

建立了高效液相色谱法快速测定参芪降糖胶囊中人参皂苷Rg1、人参皂苷Re、人参皂苷Rd含量的方法.采用3.5μm Coreshell C18核壳型分离填料(3.0 mm×150 mm)为色谱柱,分别以纯乙腈、纯水为流动相进行梯度淋洗,流量为0.43 mL/min,柱箱温度为25℃,检测波长为203 nm.人参皂苷Rg1、...     

新型抗糖尿病铬(III)配合物的合成和生物活性及机理探究

为了寻找新型的抗糖尿病分子，以苯乙双胍为前体，制备了苯乙双胍铬（III）配合物.通过元素分析、摩尔电导率、电喷雾质谱、红外光谱、紫外可见光谱和核磁共振波谱对配合物的结构进行了表征，并研究了配合物在不同温度、不同pH值下溶液的稳定性、与H₂O₂的反应性和形貌.同时，构建了糖尿病C57小鼠模型，研究了其生物活性和毒性.结果证明，配合物对其活性指标均有好的抑制作用，保留了苯乙双胍的降糖性质，对机体是无毒的，并且通过MTT（3-（4，5-二甲基噻唑-2）-2，5-二苯基四氮唑溴盐）实验说明配合物的生物相容性较好，实现了金属配合物降糖与控脂的多功能化应用.在此基础上，通过光谱法研究了配合物与胰高血糖素的相互作用，表明配合物对胰高血糖素是静态猝灭以较强的作用力结合，条件结合常数为1.29×10⁵ L·mol^-1，结合位点数约为1，初步提出了配合物的新的降糖机制.     

预富集-氢化物发生原子吸收光谱法测定饮料中的痕量铅

原子吸收光谱法测定水样中的痕量元素是应用得最广泛的方法之一[1]。有时需采用多种方法对水样中的痕量元素进行富集。其中一类方法是基于待测元素配合物可以最终定量富集于少量颗粒上,过滤收集这些颗粒,然后制成小体积的、可直接用原子吸收光谱法测定的悬浊液。特定的配位剂分     

激光剥蚀电感耦合等离子体质谱法中生物样品的元素分馏效应研究

采用213 nm-纳秒激光剥蚀系统对生物基体样品的剥蚀颗粒进行研究,优化了激光剥蚀条件.在剥蚀能量为25%,束斑直径为200 μm,剥蚀速率为20 μm/s,频率为20 Hz,载气为700 mL He + 700 mL Ar时,信号强度及稳定性最佳.以31P为内标元素,最佳剥蚀条件下,考察了56个元素的相对分馏因子.结果表明,生物基体的剥蚀颗粒相较于NIST 610 玻璃标样更大,达到3 μm;生物基体中元素分馏效应相较于玻璃基体小,大多数元素的相对分馏因子达到1.0 ±0.1.探讨了生物基体中元素分馏机理,分析了生物基体相较于玻璃基体剥蚀颗粒大,而相对分馏因子未明显增大的原因.一方面可能是粒径3 μm的颗粒进入电感耦合等离子体后能原子化;另一方面,大的剥蚀颗粒的富集效应相对较小.进一步对分馏效应的影响因素进行研究,发现分馏效应与激光剥蚀能量、激光频率和扫描速率相关,并且与元素的氧化物沸点负相关,与氧化物键能和电离能正相关.     

新型Pt／碳化树脂催化剂的制备及在微量测定有机氧元素中的应用

本文报道一种新型Pt／碳化树脂催化剂的制各方法，用该法制备的催化剂具有高分散金属和高机械强度，用于库仑法微量测定有机氧元素取得满意结果。文中对催化剂特点，Pt颗粒在催化剂表面的分布及微观形貌作了初步研究。     

无固定相分离-电感耦合等离子体质谱法在环境中痕量金属纳米颗粒分析中的应用

环境中金属纳米颗粒的分析检测不仅需要关注其浓度和化学组成,还需要对其形状、粒径和表面电荷等进行表征。此外,环境中金属纳米颗粒的分析需要解决其低赋存浓度以及复杂基质干扰的难题。无固定相分离技术与电感耦合等离子体质谱(ICP-MS)的在线联用,具有较强的颗粒分离能力和较低的元素检出限,能够快速准确地提供金属纳米颗粒的粒径分布、化学组成等信息,在金属纳米颗粒的分离检测方面表现出极大的潜能。但这一联用技术尚无法获得金属纳米颗粒物的颗粒数浓度和单个颗粒的元素信息,难以判断金属纳米颗粒涂层厚度、纯度以及颗粒的均相/异相团聚行为等。新兴的单颗粒-电感耦合等离子体质谱(SP-ICP-MS)与无固定相分离技术的在线联用,可以获得金属纳米颗粒的流体动力学粒径、元素质量计算粒径和颗粒数浓度等信息,进而弥补无固定相分离与ICP-MS在线联用技术的不足。该文介绍了流体动力色谱、毛细管电泳和场流分离3种常用无固定相分离技术的分离机制和适用检测器,着重综述了无固定相分离技术与ICP-MS/SP-ICP-MS在线联用技术的特点及其在环境金属纳米颗粒分析中的应用。关于场流分离,主要介绍了可以与ICP-MS联用的沉降场流分离和流场流分离。该文还对流体动力色谱、毛细管电泳和流场流分离与ICP-MS在线联用技术的特点进行了比较。最后,该文对无固定相分离技术与ICP-MS/SP-ICP-MS在线联用技术的发展提出了展望。     

Screening and identification of α‐glucosidase inhibitors from Shenqi Jiangtang Granule by ultrafiltration liquid chromatography and mass spectrometry

Shenqi Jiangtang Granule, a well‐known traditional Chinese herbal preparation, has been widely used for the treatment of type II diabetes mellitus. In this work, an ultrafiltration liquid chromatography with quadrupole time‐of‐flight mass spectrometry method was proposed for the rapid identification of bioactive ingredients from Shenqi Jiangtang Granule using α‐glucosidase as an example. First, the chemical profile of this preparation was clarified, including 37 saponins, 17 flavonoids, 37 lignans, and seven other compounds. After incubation with α‐glucosidase in vitro, the methanol extract with an IC₅₀ value of 0.19 mg/mL exhibited significant inhibitory activity. Then, 18 specific binding peaks were screened, and 15 peaks were identified. Among these, ten compounds were reported to have potential α‐glucosidase inhibitory activity for the first time. Subsequently, the inhibitory activities of these active compounds were evaluated by ultraviolet spectrophotometry with p‐nitrophenyl α‐d‐ glucopyranoside as a substrate. As a result, gomisin J and gomisin D exhibited stronger α‐glucosidase inhibitory activities than other active compounds with IC₅₀ values of 77.69 and 133.85 μM, respectively. The results demonstrated that the integrated ultrafiltration liquid chromatography with mass spectrometry method was an effective and powerful tool for the discovery of active ingredients in Shenqi Jiangtang Granule.     

Determination and quantification of astragalosides in Radix Astragali and its medicinal products using LC–MS

In the present study, a liquid chromatography–tandem mass spectrometry method was developed for the separation and simultaneous quantification of astragalosides I–IV in samples of Radix Astragali and a medicinal product thereof (Jinqi Jiangtang tablets). Chromatographic separation was achieved on an Agilent Eclipse XDB (ODS)‐C18 column with a mobile phase consisting of acetonitrile and 0.05% formic acid aqueous solution by use of an efficient 17‐min program. A triple quadrupole mass spectrometer was operated in positive ionization mode with multiple reaction monitoring for the detection of four astragalosides. The saponin ginsenoside Rg1 (similar structure to astralagosides) was used as an internal standard. All calibration curves showed excellent linear regressions (r² ? 0.9912) within the range of tested concentrations. The intra‐ and inter‐day variations were below 4.57% in terms of RSD. The recoveries were 94.38–103.53% with RSD of 1.39–3.58% for spiked Radix Astragali samples. The method was successfully used for the analysis of samples of Radix Astragali and Jinqi Jiangtang tablets. In conclusion, we have developed a rapid, efficient, and accurate LC–MS/MS method for the detection of astragalosides, which can be applied for quality control of Radix Astragali and related medicinal products.     

Determination of trace elements in semiconductor materials by neutron activation analysis using the radioisotope addition technique

The determination of trace elements in highly activated matrix components was carried out by neutron activation analysis using the radioisotope addition technique. The method is based on the addition to the irradiated test sample of a radioisotope which is a diffeent nuclide of the element to be determined. After separation, the chemical yield is calculated from the radioactivity added and the element is determined by an ordinary technique. Twelve elements in indium phosphide and eight elements in gallium arsenide could be determined by the method.     

Simultaneous determination of calycosin‐7‐O‐β‐d‐glucoside,calycosin, formononetin,astragaloside IV and schisandrin in rat plasma by LC‐MS/MS: application to a pharmacokinetic study after oral administration of Shenqi Wuwei chewable tablets

A rapid, sensitive and reliable high‐performance liquid chromatography–mass spectrometry (LC‐MS/MS) method was developed and validated for simultaneous quantification of the five main bioactive components, calycosin, calycosin‐7‐O‐β‐d ‐glucoside, formononetin, astragaloside IV and schisandrin in rat plasma after oral administration of Shenqi Wuwei chewable tablets. Plasma samples were extracted using solid‐phase extraction separated on a CEC₁₈ column and detected by MS with an electrospray ionization interface in multiple‐reaction monitoring mode. Calibration curves offered linear ranges of two orders of magnitude with r > 0.995. The method had a lower limit of quantitation of 0.1, 0.02, 0.1, 1 and 0.1 ng/mL for calycosin, calycosin‐7‐O‐β‐d ‐glucoside, formononetin, astragaloside IV and schisandrin, respectively. Intra‐ and inter‐day precisions (relative standard deviation) for all analytes ranged from 0.97 to 7.63% and from 3.45 to 10.89%, respectively. This method was successfully applied to the pharmacokinetic study of the five compounds in rats after oral administration of Shenqi Wuwei chewable tablets. Copyright © 2014 John Wiley & Sons, Ltd.     

广东四会十月桔种植土壤中微量元素分析

用火焰原子吸收分光光度法和阳极溶出伏安法对广东四会９个地区的十月桔及其种植土壤中１１种元素进行了测定。结果表明,四会地区十月桔富含人体有益元素,而有害元素含量极低,是一种有较高营养价值及安全的食品,土壤中各元素含量范围广,但十月桔对同一元素具有相应的富集特征。     

电感耦合等离子体光谱/质谱联机同时测定多金属结核中常量、微量、痕量元素

采用电感耦合等离子体质谱(ICP-MS)与等离子体光谱(ICP-OES)联机同时测定多金属结核样品中常量、微量、痕量元素。样品经高压密封溶样弹消解后,一次气动雾化进样,ICP-OES测定常量和微量元素,ICP-MS测定微量和痕量元素。详细探讨了不同浓度范围元素的测定方式、元素分析信号的采集模式、多原子离子干扰的校正因子。采用ICP-MS与ICP-OES二种方式同时测定Co、Cu、Ni、Zn、V、Ba、Sr,分析结果表明具有较好的一致性。所建立的ICP-MS与ICP-OES联机检测技术用于多金属结核标准样品的分析(Nod-A-1,GSPN-1,GSPN-2,GSPN-3),分析结果与推荐值符合,相对标准偏差小于10％。     

溪黄草微量元素含量及其溶出量分析

用等离子体原子发射光谱法对溪黄草微量元素的含量进行了测定,溪黄草含有１８种元素,其微量元素的水溶出量与溪黄草的提取方法有关。     

标准溶液配制用碳酸锂纯物质中杂质含量的测定

从高纯碳酸锂中杂质含量测定出发,研讨了标准溶液配制用原料的杂质测定方法,首先利用电感耦合等离子体质谱(ICP-MS)法对高纯碳酸锂进行半定量分析,再依据半定量分析结果选择ICP-MS、电感耦合等离子体原子发射光谱(ICP-AES)法、原子吸收光谱(AAS)法等方法对相应元素(杂质含量0.001%)进行定量分析,通过扣除杂质含量得出高纯碳酸锂纯度大于99.991%。从而建立了一个准确、高效,覆盖元素种类多的高纯物质中杂质含量的分析方法     

青黛中微量元素含量测定分析

用原子吸收分光光度法测定了青黛中的7种微量元素。结果表明,青黛中含有丰富的人体必需的微量元素和极微量的有害元素镉和铅。