微波消解-电感耦合等离子体-质谱法连续测定啤酒花中的11种微量元素

使用带预消解步骤的微波消解方法处理样品,电感耦合等离子体-质谱法结合碰撞池技术(CCT,Collision Cell Technology)连续测定了啤酒花样品中的11种微量元素.方法各元素相关系数均大于0.9995,相对标准偏差RSD＜5％,回收率为82.0％-112.0％.     

微波消解电感耦合等离子体-质谱法测定面粉中的铝

面粉样品经微波消解后,以⁴⁵Sc为内标元素校准基体效应及信号漂移,用电感耦合等离子体.质谱法直接测定,外标法绘制校准曲线进行定量。测定面粉中铝的检出限为0.25mg/kg,线性良好,相关系数r=0.9999,相对标准偏差1.25%—3.03%,加标回收率在93.9%—103.5%之间。该方法灵敏快速,干扰小,重现性好,能满足面粉中铝含量测定的要求。     

微波消解-电感耦合等离子体质谱法同时测定海藻羊栖菜中的微量元素

采用微波消解-电感耦合等离子体质谱(ICP-MS)法测定海藻羊栖菜中Co、Pb、Cd、As、Cu、Zn、V、Cr 8种微量元素,对样品的前处理条件进行了探讨,选用Li、Sc、Ge、Y、In、Tb、Bi 7种元素作内标液校正基体效应和信号漂移,该方法对8种待测元素的检出限分别为0.007-0.042μg/g,相对标准偏差为0.42%-2.56%,标准物质测定回收率为92.5%-106.5%,对标准物质样品分析的结果与所给参考值吻合.方法快速、简便、准确,适合常规分析.     

微波消解/电感耦合等离子体质谱测定鹿骨粉中微量元素

采用HNO₃-H₂O₂ 微波溶样、电感耦合等离子体质谱法测定了鹿骨粉中的微量元素。在优化的实验条件下,方法的检出限(3σ, n=11)为0.000 6～1.498 ng·mL-1;标准加入回收率为91％～109％,相对标准偏差为1.7％～6.8％。对国家标准物质样品分析的结果与所给参考值吻合。     

电感耦合等离子体-质谱法同时测定雷公藤中常量及微量元素

采用微波消解法对雷公藤进行消解制样,用电感耦合等离子体-质谱法(ICP-MS)同时测定了其常量及微量元素,并研究了常量及微量元素的含量特征.方法的相对标准偏差(RSD)＜9％,回收率在90.0％-103.0％之间.结果表明,中药雷公藤中含有比较丰富的K、Ca、Fe、Mg、Mn、Zn等元素,对人体有害的微量元素Pb、Cd...     

微波消解ICP-MS测定唐古特乌头中的多种微量元素

采用HNO3-H2O2混合酸体系微波消解及电感耦合等离子体-质谱法,消解唐古特乌头样品,测定其中Mn、Fe、Co、As、Ni、Se、Cu、Zn、V和Cr共10种微量元素。探讨了样品消解的条件,通过加标回收实验,回收率为94.08%—103.50%,验证了分析数据的可靠性。结果表明,该法具有快速、简便、准确度高、能同时分析多元素的优点,结果令人满意。     

微波消解-电感耦合等离子体质谱法同时测定烟草中27种元素

在烟草中的有机和生物活性成分被鉴定出来之后,分析和鉴别其中的无机元素就变得非常重要。采用电感耦合等离子体质谱法同时测定了烟叶中Be,Na,Mg,K,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,As,Se,Sr,Mo,Ag,Cd,Sn,Cs,Ba,Hg,Tl,Pb,Th和U共27种元素。样品的前处理采用硝酸和过氧化氢混合溶液。通过在线加入内标液的方法来校正由于基体效应和信号漂移对测量所造成的影响,内标选用锗、铟和铋3种元素。方法的回收率为93.64%～108.9%,检出限为0.356 3 ng·L-1～1.725 μg·L-1,相对标准偏差1.28%～9.18%。实验结果表明该方法能满足痕量分析的要求。     

微波消解-电感耦合等离子体-质谱法测定大米中的铅、镉、汞和砷

应用微波消解-电感耦合等离子体-质谱法(ICP-MS)一次进样同时测定大米中的铅、镉、汞、砷含量.采用8mL硝酸+2mL过氧化氢的微波消解体系,消解后无需赶酸,定容后直接用ICP-MS测定.实验发现,运用该方法干扰少,速度快,多元素同时分析,重现性好,准确度高.该方法的回收率分别为:Pb:100.9％、Cd:90.1％、Hg:86.1％、As:92.8％.Pb、Cd、Hg、As方法检出限均为0.001ng/mL.     

电感耦合等离子体质谱法快速测定中药中的微量元素

采用电感耦合等离子体-质谱法测定了中药中微量元素K、Ca、Mn、Cu、Zn、的含量.探讨了微量元素与中药疗效之间的联系.选取样品中的大青叶对各测定元素做了加标回收率实验,回收效果良好;并选取金银花做精密度实验,RSD均小于2％.     

微波消解-ICP-AES测定植物样品中多种微量元素

用微波消解仪消解植物样品,ICP-AES同时测定样品中硼、硫、磷、钾、钠、钙、镁、铜、锌、锶、钡、锰、铁等13个元素。方法检出限为0.087-6.03μg/g,精密度（RSD%,n=12）为0.49%—2.28%。对大米、茶叶、豆角、紫菜、花粉、黄芪国家一级标准物质进行测定,测定值与推荐植相符。结果表明,该方法可以满足植物样品中微量元素测定的要求。     

电感耦合等离子体质谱法测定饮用水中6种痕量重金属元素

采用电感耦合等离子体质谱(ICP-MS)法同时测定饮用水中的镉、铬、铅、锌、铜、镍6种元素的含量.对仪器工作参数进行了优化,选取45Sc,72Ge,115In, 209Bi作为测定元素的内标元素,有效克服了基体效应、接口效应及仪器波动所产生的影响,利用八极杆碰撞/反应池技术,消除多原子离子对待测元素的干扰.测定元素校准曲线的相关系数都在0.999 7以上,各元素的检出限在0.70～77.0 ng·L-1之间,相对标准偏差(RSD)介于0.47%～1.69%之间.测定标准参考物GBW08607,测定值均在标准值范围内.对4个地区的饮用水进行了检测,样品加标回收率为92%～108%.该方法具有简便、快速、准确、稳定的特点,可作为饮用水中痕量元素检测的可靠方法.     

电感耦合等离子体质谱法测定高钝镉中的杂质元素

采用电感耦合等离子体质谱光测定离纯镉中的杂质元素。讨论了镉基体的谱线干扰,比较了镉基体产生的多原子离子的干扰程度,该干扰按ＣｄＨ、ＣｄＯ、ＣｄＯ２、ＣｄＡｒ、ＣｄＯＨ和ＣｄＯＨ２顺序递减。研究了不同浓度镉基体对分析物信号的抑制或增强效应,镉的浓度大于０．２５ｇ·Ｌ＾－１时,对质量数小于１００的分析物的信号强度产生抑制,而以质量数大于１５０的分析的信号强度产生增强,采用＾８９Ｙ和＾２０９Ｂｉ作内标分     

Microfluidic chip-inductively coupled plasma mass spectrometry for trace elements and their species analysis in cells

Abstract

Accurate identification and quantification of trace elements and their species in cells is an important prerequisite for the exploration of their physiological function and related mechanisms of process involving trace elements/species in human body. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful analytical instrument for trace elements detection, while it still suffers from insufficient limits of detection, interference from complex cell matrix, and incompatible sample consumption in cells analysis. Microfluidic chips which possess advantages of low sample/reagent consumption, rapid analysis speed and high spatial resolution provide perfect miniaturized and integrated platforms for cell analysis. In this article, microfluidic chip-ICP-MS techniques for trace elements and their species analysis in cells were reviewed. Both chip-based pretreatment techniques (e.g., magnetic solid phase microextraction (MSPME), monolithic capillary microextraction (MCME), liquid phase microextraction (LPME)) including chip-based array microextraction techniques for trace elements and their species analysis and droplet chip for single cell analysis were introduced. The newly developed methods of microfluidic chips in combination with ICP-MS for trace elements and their species analysis in small numbers of cells and even single cell were critically discussed, including chip-based MSPME/MCME/LPME-(electrothermal vaporization-ICP-)MS, on-line chip-based array MSPME/MCME-ICP-MS, on-line chip-based array MSPME-high performance liquid chromatography-ICP-MS and online droplet chip-time-resolved ICP-MS. These methodologies were demonstrated with high sensitivity, high throughput, good matrix resistance and low sample/reagent consumption, contributing to the quantification of trace elements/species in cells and even single cells. Relevant 20 references are included herein, and the development trend of microfluidic chip-ICP-MS techniques for cells analysis is prospected.     

Determination of arsenic species in mainstream cigarette smoke based on inductively coupled plasma mass spectrometry

In this work, arsenic species in mainstream cigarette smoke condensates was systemically studied with inductively coupled plasma mass spectrometry. A single particle inductively coupled plasma mass spectrometry was utilized for analysis of the physical forms of arsenic, and no particle arsenic was observed in mainstream cigarette smoke condensates. The solvent extraction experiments proved that the water-soluble arsenic was the main species in mainstream cigarette smoke condensates, which was consistent with the result of single particle inductively coupled plasma mass spectrometry. Furthermore, speciation of arsenite, arsenate, monomethylarsonic acid, and dimethylarsinic acid was investigated using high performance weak anion exchange chromatography coupled with inductively coupled plasma mass spectrometry detection. The developed high performance liquid chromatography coupled inductively coupled plasma mass spectrometry method was successfully applied to the determination of arsenic species in mainstream cigarette smoke condensates with satisfactory recoveries. Four arsenic species were detected in the mainstream cigarette smoke condensates from four brands of commercial available cigarettes, and there was a great difference between the arsenic content and composition among the different brands of cigarettes. It is found that arsenate was the main species in all tested cigarette samples.     

激光剥蚀-电感耦合等离子体质谱测定植物样品中的元素

采用193 nm准分子激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)对标准植物粉末样品(GBW07602-GBW07603灌木枝叶、GBW07604杨树叶、GBW07605茶叶、GBW08514烟草)中13种元素(Li,B,Na,Mg,Al,K,Ca,Cr,Mn,Fe,Ni,Cu,Ba)进行定量测试.向植物粉末样...     

凝胶电泳与激光剥蚀-电感耦合等离子体质谱联用测定蛋白质中微量元素的应用进展

介绍了凝胶电泳(GE)和激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)联用测定蛋白质中微量元素的方法,对蛋白质分离、凝胶处理,包括染色及干燥,和检测过程中的定量校正等技术问题做了详述,并综述了LA-ICP-MS在硒蛋白、磷酸化蛋白及金属蛋白分析中的应用,指出了这种方法在蛋白质中微量元素检测中存在的问题和发展方向。     

激光剥蚀电感耦合等离子体质谱鉴别蓝色圆珠笔色痕

建立了法庭科学中蓝色圆珠笔色痕的激光剥蚀电感耦合等离子体质谱鉴别方法。对95种不同来源的蓝色圆珠笔进行了分析,依据所含金属元素种类的差别将95种圆珠笔分为34类,其中26类圆珠笔根据元素种类的差别可直接区分,其余8类依据元素间响应值之比进行区分,对字痕载体纸张的考察结果表明了纸张对检测结果无影响。实验结果表明方法重现性良好,精密度10%,与传统分析技术相比,本方法可获得更好的鉴别结果,95种蓝色圆珠笔中有88种可使用该方法有效鉴别。该方法简便快速、精密度良好、对样本宏观无损,适合法庭科学对蓝色圆珠笔鉴定的需要。     

Determination of trace BrO3- and Br- in Chinese patent drugs, waters and beverages by ion chromatography coupled with inductively coupled plasma mass spectrometry

In the present study, a method for determination of BrO3- and Br- using ion chromatograghy coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS) was developed. BrO3- and Br- were separated on a Hamilton PRP X-100 (150 x 4.1 mm, 10 microm) column guarding with a On-guard II RP (4 x 50 mm) column with 10 mmol x L(-1) NH4NO3 eluent solution at 2 mL x min(-1). By using 200 microL sample loop, the detection limits for BrO3- and Br were 0.35 and 0.36 microg x L(-1), respectively. BrO3- had good linearity in the range 4.8-160.0 ng x L(-1). The standard solution linear equation was y = 250.31x-45.43, and R2 = 0.9999. Br had good linearity in the range 4.2-140.0 ng x L(-1). The standard solution linear equation was y = 186.84x-127.10, and R2 = 0.9994. Recoveries of spiked samples were 98.9%-109.5% and 97.4%-106.1%, respectively. The samples included various kinds of Chinese patent drugs, waters, and beverages. Among them, 14 bottled drinking waters and 2 kinds of tap waters were found containing BrO-, while other samples were under BrO3- detection limit. Br- was detected in all samples.     

Determination of the spatial distribution of trace elements in stainless steel by imaging microprobe secondary ion mass spectrometry

Imaging microprobe secondary ion mass spectrometry (SIMS) using a liquid metal ion source (LMIS) has been used to determine the spatial distribution of metal ions in stainless steel. This scanning ion microprobe is used to achieve high resolution chemical maps of the surface of a sample. For conductive samples such as stainless steel, the practical spatial resolution approaches 0.2 μm and the sensitivity varies with the ion of interest. We have obtained important information relating to the distribution of surface contaminants, segregation, and corrosion phenomena of the elements in these alloys. In this report we hope to demonstrate the usefulness of this important new technique by describing its capabilities and by reviewing data obtained from two separate studies involving stainless steel.

Significant findings obtained in these mapping experiments were:

• . Stainless steel 316 tubing, which had been found previously to be catalytically active, showed remarkable differences between the used and unused samples. Sodium, potassium, and hydrocarbons were found to exist in agglomerations (islands) in the unused tubing, but were very well distributed in the used tubing.

• . A used stainless steel impeller was found to be inhomogeneous with respect to iron and chromium. The surface was entirely covered by chlorine, which is believed to be responsible for the corrosion. Water and elevated levels of chloride ion were found inside numerous scratches or fissures covering the surface. The unused stainless steel showed no signs of streaks or segregated metal regions, and was free from fissures.

     

Standardless analysis of solids by mass spectrometry with inductively coupled plasma

The possibility of the standardless mass spectrometric analysis of the elemental composition of solids has been discussed. The effect of each stage of the laser plasma expansion on the formation of the coefficient of relative sensitivity of elements in the sample has been studied theoretically and experimentally. It has been shown that the stages of ionization and detection make the main contribution to the formation of the coefficient of relative sensitivity. It has been proposed to separate dissociation and ionization processes in time and/or in space. To compensate for the energy spread of ions at the output of the analyzer, a circuit has been proposed for aligning the energy of ions before their detection.