羊红膻中微量元素含量的测定

采用高分辨全谱直读电感耦合等离子体发射光谱仪测定了羊红膻(Pimpinella thellungianaWolff)药材地上与地下不同部位中含Cu、K、Na、Fe、Se、Mg、As、Ca、Cd、Cr、Mn、Ni、P、Pb和Zn等15种微量元素含量,并进行了比较。结果表明,重金属As和Pb几乎检测不到,K含量均高;同时也为羊红膻药理作用及临床用药提供科学依据。     

火焰原子吸收光谱法测定赣南脐橙中6种微量元素含量

将赣南脐橙经硝酸和高氯酸消化后,在样品中加入氯化镧作为释放剂以消除共存离子的干扰,采用火焰原子吸收光谱法测定了Ca、Mn、Zn、Fe、Cu和Pb元素的含量。结果表明,标准加入法的回收率为．96．58％～104．31％,10次平行测定结果的相对标准偏差RSD均小于2％。该法灵敏度高、操作简便快速,结果准确,重现性好。可见赣南脐橙中各元素含量差异显著,其中ca的含量比较丰富,Mn、Fe和zn的含量中等,含有人体必需的微量元素,而对身体有害的元素如P11含量却相当低,这说明赣南脐橙具有一定的药用和经济价值,为进一步探讨赣南脐橙开发利用提供实际依据。     

微波消解-FAAS法测定大别山区三种中药中的微量元素

采用微波消解-火焰原子吸收光谱(FAAS)法对大别山区3种中药(何首乌、黄精和拐枣)中的微量元素进行测定。用微波消解仪处理样品,对消解条件及消解程序进行优化,在最佳微波消解条件下,结合FAAS法测定上述3种中药中Ca、Mg、Cu、Zn、Fe、Mn 6种元素的含量。结果表明,微波消解的最佳条件为:何首乌和拐枣采用HNO3-H2O2混酸体系,配比分别为5∶2和5∶3,固液比1∶20,最高功率(700W)时的保温时间分别为8min和6 min;黄精采用HNO3-HCl,混酸体系,配比5∶2,固液比1∶28,保温时间为8 min。所建立的定量分析方法回收率为95.63%～101.36%,相对标准偏差小于3.0%,线性相关系数大于0.999,方法检出限为0.18～2.20 ng/mL。3种中药中均含有丰富的微量元素,尤其是黄精中Fe、Ca和Mn的含量较高;何首乌中Mg、Zn和Fe含量相对较高;拐枣中Fe和Ca含量相对较高。研究结果可为上述3种中药中微量元素的含量与其药效的相关性提供科学依据。     

西安市某辖区2～6岁儿童全血样品微量元素含量状况调查

摘要对西安市某辖区妇幼保健站及多家幼儿园920名2～6岁身体健康儿童的全血样品进行微量元素检测,统计得到该区域正常儿童微量元素的含量范围,为准确了解西安地区某区域2-6岁正常儿童体内微量元素正常含量提供了参考数据。     

化工工人体内微量元素积累与健康的关系

论述了化工作业工人长期接触有害元素会引起体内有害元素积蓄，微量元素平衡失调，产生潜在的职业危害，建议定期对临床尚未发现中毒现象的作业工人进行体内微量元素情况监控，以预防职业中毒。并提出采用适当补充某些必需元素的方法，可预防这种危害。     

脑卒中患者血清中8种必需微量元素水平的研究

１１０例脑卒中患者血清中铁，锌，铜，锰，硒，铬，钴，镍的含量水平与对照组比较，结果显示：１．血清的，铜和铬的含量升高，锌，钴和镍的含量降低，两者之间的差异均有高度显著性，Ｐ〈０．０１；２．血清锰和硒的含量与对照组差异无显著性，Ｐ〉０．０５；３．在临床上述元素含量变化可用于脑座中的辅助诊断和治疗。     

微波消解-ICP-MS法测定药用明胶空心胶囊中微量重金属元素

采用微波消解技术,建立了一种电感耦合等离子体质谱法测定明胶空心胶囊中Cr,Co,Ni,Cu,Zn,As,Cd,Hg和Pb 9种微量重金属元素的方法。确定了微波消解仪和等离子体质谱仪的最佳操作参数,研究共存离子的干扰和消除方法,选择了各元素的测定同位素,以Ge,Rh和Tl为内标补偿基体效应,建立了样品测定方法。应用拟定的方法测定了不同生产厂家、不同批次的空心胶囊中微量重金属的含量。方法对试样中各元素测定的相对标准偏差为1.5%~14.1%,加标回收率在90.0%~102.0%。结果表明,方法简便、快速、灵敏,满足于空心胶囊中9种重金属元素的测定要求。     

Double-ion imprinted polymer @magnetic nanoparticles modified screen printed carbon electrode for simultaneous analysis of cerium and gadolinium ions

A typical, reproducible, and rugged screen printed carbon electrode, modified with dual-ion imprinted beads, was fabricated employing the “surface grafting from” approach. For this, the acyl chloride functionalized magnetic nanoparticles were first immobilized and chemically attached with a typical functional monomer (but-2-enedioic acid bis-[(2-amino-ethyl)-amide]) on the electrode surface. This was subsequently subjected to the thermal polymerization in the presence of template ions (Ce(IV) and Gd(III)), cross-linker (ethylene glycol dimethacrylate), initiator (AIBN), and multiwalled carbon nanotubes. The modified sensor was used for the simultaneous analysis of both template ions in aqueous, blood serum, and waste-water samples, using differential pulse anodic stripping voltammetry which revealed two oxidation peaks for respective templates with resolution as much as 950 mV, without any cross reactivity, interferences and false-positives. The detection limits realized by the proposed sensor, under optimized conditions, were found to be as low as 0.07 ng mL⁻¹ for Ce(IV) and 0.19 ng mL⁻¹ for Gd(III) (S/N = 3) that could eventually be helpful for lanthanide estimation at stringent levels.     

Cheminformatics in MS-based environmental exposomics: Current achievements and future directions

Compound annotation using MS/MS data is the major bottleneck in interpretation of mass spectrometry data during non-targeted screening and suspect screening exposomics studies. Apart from compound identification using available databases or mass spectral libraries, the true challenge comes when completely new compounds have to be identified. Along with recent advances in MS instrumentation that set grounds to a new revolutionary age in environmental exposomics, a multitude of cheminformatics annotation approaches has been developed. Herein, we review the basic principles of the cutting-edge cheminformatics MS-based approaches employed in eco-exposome annotation.We give a solid background discussing the eco-exposome concept in relation to the advances in MS instrumentation, and define the three crucial cheminformatics tasks used in the eco-exposome annotation: molecular formula assignment, compound prioritization and compound annotation. The basic principles of compound annotation are discussed, which are based on three approaches of utilizing structural information inherent to MS data. These involve direct, indirect and joint annotation approaches. We assess their performance through the ability to annotate eco-exposome constituents. We discuss future perspectives and give directions to new annotation strategies and performance evaluation protocols aiming to solve current issues hampering the incorporation of cheminformatics annotation approaches in regular eco-exposome annotation workflows.     

在线固相萃取-液相色谱-串联质谱法检测蘑菇中毒患者尿液中痕量α -鹅膏毒肽

建立了在线固相萃取-液相色谱-串联质谱（online SPE-LC-MS/MS）测定蘑菇中毒患者尿液中痕量α -鹅膏毒肽的分析方法。样品经甲酸酸化的乙腈-甲醇（5：1,v/v）沉淀蛋白质,反相液液微萃取去除样品提取液中的有机溶剂,毒素经ODS微柱（5 mm×2.1 mm,5 μm）在线SPE净化,XBridge^TM BEH C₁₈ 色谱柱（150 mm×3.0 mm,2.5 μm）分离,MS/MS测定。采用基于定量环的快速阀切换技术作为在线SPE和LC-MS/MS模块的接口,使得两个分离模块互相独立,无论是流动相还是压力,都不会互相干扰,保证了系统的稳定性;在线系统的精准净化,有效消除了后续质谱检测的基质效应,确保了尿液中痕量水平α -鹅膏毒肽的定性定量检测。尿液中α -鹅膏毒肽在0.1~50 μg/L范围内线性关系良好,相关系数（r ² ）为0.9983;检出限（LOD）为0.03 μg/L;α -鹅膏毒肽的加标（0.1、2.0和20 μg/L）平均回收率为84.3%~91.7%,相对标准偏差（RSD）为3.8%~7.2%。体内鹅膏毒肽代谢迅速,生物基质中痕量水平毒素的检测是其中毒实验室鉴定的主要难题,通过实际样品检测,证明该法操作简单,准确、灵敏;溶剂沉淀蛋白质和反相液液微萃取去除有机相和脂溶性基质的简单操作,可以作为水溶性毒素在线SPE-LC-MS/MS检测时快速且有效的配套前处理方法;基于在线SPE精准净化技术,可以实现尿液中α -鹅膏毒肽的高灵敏度测定（LOD为0.03 μg/L）,解决了中毒时患者体内痕量水平α -鹅膏毒肽定性确证的难题,部分患者α -鹅膏毒肽中毒实验室鉴定的时间可以扩展到90 h以上;同时,痕量水平的定量检测技术,可以为中毒后迅速代谢的α -鹅膏毒肽在体内的剂量反应关系研究提供可靠的技术支撑。