氧化镁烧结-电感耦合等离子质谱法测定冰铜中的铼

本文建立了一种利用电感耦合等离子体质谱法（ICP-MS）测定冰铜中铼的方法。样品经氧化镁烧结,热水浸取法处理,溶液经732强酸型阳离子交换树脂处理交换去除干扰离子,实现了ICP-MS直接测定冰铜中的铼。实验结果表明,在最佳试验条件下,方法的检出限可低至0.010mg/t,加标回收率为92.00%~104.00%,测定结果的相对标准偏差（RSD,n=7）小于5%,测定结果令人满意。由此可见,该方法精密度高,准确度高,可用于冰铜中铼的测定。     

Inductively coupled plasma-mass spectrometry for the determination of elements and elemental species in food: a review

Inductively coupled plasma-mass spectrometry (ICP-MS) has definitely emerged as a powerful technique for total element determination and as a sensitive and selective detector in hyphenated methods for speciation analyses of elements in foods. In this review, the analytical challenges of elemental analysis of food and agricultural matrixes are discussed and several applications are examined. Selected examples illustrate the analytical approaches being used so far to address specific issues in various areas of food and nutrition research. The applications discussed include studies on dietary intake, element metabolism in man, transfer of elements through the food chain, effects of food processing and domestic preparation, and authenticity and origin assessment. The use of ICP-MS in the field of analytical quality assurance, food control, evaluation of food contact materials, and radionuclide contamination is also examined. Finally, the hyphenated techniques with ICP-MS detection used for elemental speciation in food are reviewed, and an overview of the main applications currently in the literature is presented. Throughout, recent trends and analytical developments likely to have a major impact on food-related areas are highlighted.     

Inductively coupled plasma mass spectrometry and electrospray mass spectrometry for speciation analysis: applications and instrumentation

To gain an understanding of the function, toxicity and distribution of trace elements, it is necessary to determine not only the presence and concentration of the elements of interest, but also their speciation, by identifying and characterizing the compounds within which each is present. For sensitive detection of compounds containing elements of interest, inductively coupled plasma mass spectrometry (ICP-MS) is a popular method, and for identification of compounds via determination of molecular weight, electrospray ionization mass spectrometry (ESI-MS) is gaining increasing use. ICP-MS and ESI-MS, usually coupled to a separation technique such as chromatography or capillary electrophoresis, have already been applied to a large number of research problems in such diverse fields as environmental chemistry, nutritional science, and bioinorganic chemistry, but a great deal of work remains to be completed. Current areas of research to which ICP-MS and ESI-MS have been applied are discussed, and the existing instrumentation used to solve speciation problems is described.     

电感耦合等离子体质谱分析

简要综述了我国学者近10年来在电感耦合等离子体质谱(ICP-MS)分析领域的研究工作.在ICP-MS新进样技术和ICP-MS生物分析方法学研究方面,我国科研人员开展了开拓性的研究工作,在元素形态分析和金属组学研究方面富有特色.ICP-MS仪器/部件的设计研制尚待加强;ICP-MS成像研究和在实际生命体系的应用有待进一步强化.     

Selenium speciation analysis using inductively coupled plasma-mass spectrometry

Selenium exists in several oxidation states and a variety of inorganic and organic compounds, and the chemistry of selenium is complex in both the environment and living systems. Selenium is an essential element at trace levels and toxic at greater levels. Interest in speciation analysis for selenium has grown rapidly in this last decade, especially in the use of chromatographic separation coupled with inductively coupled plasma-mass spectrometry (ICP-MS). Complete characterization of selenium compounds is necessary to understand selenium's significance in metabolic processes, clinical chemistry, biology, toxicology, nutrition and the environment. This review describes some of the essential background of selenium, and more importantly, some of the currently used separation methodologies, both chromatographic and electrophoretic, with emphasis on applications of selenium speciation analysis using ICP-MS detection.     

On-line coupling of gel electrophoresis and inductively coupled plasma-mass spectrometry

The on-line coupling of gel electrophoresis with inductively coupled plasma-mass spectrometry (GE-ICP-MS) is a powerful tool for simultaneous separation, detection and quantification of bio-molecules, and has been applied to the determination of phosphorus in DNA, phosphoproteins, and phosphopeptides, gold in nano-particles, iron in metalloproteins, and iodine in aerosols, and cisplatin-oligonucleotide interactions. However, since the first report in 2005, relatively few papers have been published, perhaps reflecting the lack of familiarity with the benefits of this promising methodology. So, here for the first time, we critically review the applications of GE-ICP-MS, and explore the advantages and the limitations of the technique for various applications. Such scrutiny may be useful in not only the development of the technique but also highlighting its potential in proteomics, genomics and metallomics.     

Effects of sampler-skimmer separation in inductively coupled plasma-mass spectrometry

The effects of varying the sampler-skimmer spacing in an inductively coupled plasma-mass spectrometer are illustrated. The signals for a number of species were monitored including background ions (ArN⁺, ArO⁺, ArOH⁺, Ar₂⁺, Ar₂H⁺), background continuum, analyte ions (Cu⁺, Ce⁺, La⁺), analyte oxide ions (CeO⁺, LaO⁺), and matrix induced ions (ArNa⁺). As the sampler-skimmer spacing is increased over that normally used, the signal for some species decreases in intensity while the signal for others increases in intensity. There is a wide range of differential behavior and in some cases the signal changes are quite dramatic.

In addition to presenting results for an Ar plasma, measurements are also presented for a N₂-Ar mixed gas plasma. For some species, the signal changes observed when the sampler-skimmer spacing is increased are quite different with the N₂-Ar mixed gas plasma than with the Ar plasma and are, in some cases, opposite to signal changes observed with the Ar plasma. It appears that a larger sampler-skimmer spacing is more appropriate for a N₂ mixed gas plasma than the spacing normally used for a pure Ar plasma. Finally the effect of sampler-skimmer spacing on matrix effects is presented and it appears that matrix effects are not induced in the zone between the sampler and the skimmer.     

基于电感耦合等离子体质谱的生物分析

ESI/MALDI-MS在生物分子结构鉴定方面的优势是ICP-MS无法匹敌的;另一方面,针对生物分子的定量分析,ICP-MS因化学选择性和生物特异性元素标记策略的发展而极具优势。它们的联合使用必将为生物分析(特别是定量蛋白质组学和金属组学研究)提供解决问题的新途径,这时我们需要一个化学集成器(chemical hub)针对目标生物分子或细胞正交集成运用ESI/MALDI-MS和ICP-MS而不是简单地物理平行使用,使得ICP-MS知道定量的是何种生物分子或细胞,这对未知生物分子或细胞的发现和绝对定量十分重要。     

Automatic selection of internal standards in inductively coupled plasma-mass spectrometry

The automatic selection of internal standards in inductively coupled plasma-mass spectrometry was performed using a cluster analysis algorithm. The samples contained 25 analytes, spanning the atomic mass and ionization potential ranges, and a single interfering element. The interferents examined were Na, Mg, K, Zn, Ba, and Pb. The cluster analysis algorithm used kinetic energy, ionization potential, oxide bond strength, hydride bond strength, and electronegativity, to group the analytes. These variables were weighted differently in the various matrices. The performance of the clustering method and selection of internal standards was good for most analytes in the various matrices.     

Uranium colloid analysis by single particle inductively coupled plasma-mass spectrometry

Uranium single particle analysis has been performed by inductively coupled plasma-mass spectrometry (ICP-MS) and the performances are compared with that provided by scanning electron microsopy and single particle counting. The transient signal induced by the flash of ions due to the ionisation of an uranium colloidal particle in the plasma torch can be detected and measured for selected uranium ion masses (²³⁸U⁺, ²³⁵U⁺ or ²⁵⁴[²³⁸U¹⁶O]⁺) by the mass spectrometer. The signals recorded via time scanning are analysed as a function of particle size or fraction of the studied element or isotope in the colloid phase. The frequency of the flashes is directly proportional to the concentration of particles in the colloidal suspension. The feasibility tests were performed on uranium dioxide particles. The study also describes the experimental conditions and the choice of mass to detect uranium colloids in a single particle analysis mode.     

Determination of trace lead by hydride generation-inductively coupled plasma-mass spectrometry

A newly developed hydride generation-inductively coupled plasma-mass spectrometry (HG-ICP-MS) system was employed to determine trace amounts of lead in geological and biological samples. Laboratory-made single-stage and double-stage gas-liquid separators (GLSs) were investigated in order to replace the consumable membrane-GLS. Possible reasons were given why double-stage GLSs were superior over the single-stage ones according to the factors such as GLS volume and configuration, carrier gas inlet mode and flow rate. Interferences in liquid and vapor phase from concomitant ions and their products were investigated employing different flow mani-folds. Memory effects contributed to the blank values, but could be reduced employing a special wash protocol. Internal and external standardization were combined to improve the accuracy of the method, with bismuth as the internal standard according to its similarity with lead in the HG-ICP-MS system. Compared with ICP-MS and hydride generation-atomic fluorescence spectrometry (HG-AFS) methods, the system performance of HG-ICP-MS was characterized with improved detection limit to 0.002 ng/ml and acceptable short- and long-term stabilities. The linear dynamic range of this method was up to 50 ng/ml lead. Three Chinese national certified reference materials: poplar leaves, human hair and copper ore, were analyzed for method validation, and the results agreed well with the certified values. At last, the method was also employed to determine wide range of lead concentrations in lightweight limestone and nervous tissue samples from infants of albino rats with recoveries between 95 and 105% (n=10).     

Background spectral characteristics in direct sample insertion-inductively coupled plasma-mass spectrometry

An extensive set of background spectra are presented for a direct sample insertion-inductively coupled plasma-mass spectrometer (DSI-ICP-MS) system. These include spectra of a dry plasma (i.e. one in which no sample or solvent is introduced) and background spectra for DSI sample probes such as graphite, Mo and Ta cups as well as a W wire loop. Compared to the background spectra measured when aqueous solutions are nebulized into the plasma the DSI background spectra are considerably simpler. Primarily due to the elimination of water in DSI systems there is a significant reduction and even elimination of numerous background species, particularly those containing oxygen and hydrogen. In addition, the DSI sample probes themselves do not add any complex species to the spectral background.     

Thorium colloid analysis by single particle inductively coupled plasma-mass spectrometry

Thorium colloid analysis in water has been carried out by a single particle mode using inductively coupled plasma mass spectrometry (ICP-MS). The flash of ions due to the ionisation of a thorium colloidal particle in the plasma torch can be detected and measured in a time scan for ²³²Th⁺ or ²⁴⁸[ThO]⁺ according to the sensitivity required by the mass spectrometer. The peaks of the recorded intensity of the MS signal can be analysed as a function of the particle size or fraction of the studied element in the colloid phase. The frequency of the flashes is directly proportional to the concentration of particles in the colloidal suspension. After discussing Th colloid detection, on the basis of the intensity of the ion flashes generated in the plasma torch, tests were performed on thorium dioxide colloidal particles. This feasibility study also describes the experimental conditions and the limitation of the plasma design to detect thorium colloids in a single particle analysis mode down to about 10 fg.     

电感耦合等离子体质谱法测定地球化学样品中镉

采用HF-HClO4-HNO3-H2SO4分解样品,王水提取,选用4个国家一级标准物质制备成标准系列校准,ICP-MS法直接测定地球化学样品中的Cd。选择103Rh为内标,确定了仪器的最佳分析条件,研究了Zr,Sn对Cd的干扰,选择114Cd作为测定同位素,采用数学公式校正了Sn对Cd的同质异位素干扰,方法检测限(3s)为6.3×10-3μg/g,RSD(n=12)为3.9%～6.6%。经国家一级标准物质验证,测定值与标准值吻合较好。该方法适用于地球化学样品中的微量Cd的测定。     

Multielemental analysis of food and agricultural matrixes by inductively coupled plasma-mass spectrometry

The suitability of quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) for multielemental analysis of food following microwave closed vessel digestion of samples was evaluated in relation to analytical challenges presented by some major food and agricultural matrixes. Fifteen key analytes (Al, As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Se, Sn, V, Zn) were determined in 9 reference materials representative of 3 major groups of staple foods (cereals, seafood, and meat). For all measurements, the method of external calibration was used and Rh was selected as internal standard. Matrix-induced interferences were evaluated for each material, and suitable methods to overcome them were applied. Spectral interferences caused by C, Cl, and Ca content of digestates were quantitated and corrected by entering a simple system of mathematical correction equations into the instrument software before each analytical run. Full mastering of interferences together with adoption of a series of measures to control the reliability of analytical measurements produced accurate results for all the analytes. A standard analytical protocol is outlined for the benefit of both research and routine high-throughput laboratories that perform ICP-MS analyses of food.     

Using inductively coupled plasma-mass spectrometry for calibration transfer between environmental CRMs

Multielement analyses of environmental reference materials have been performed using existing certified reference materials (CRMs) as calibration standards for inductively coupled plasma-mass spectrometry. The analyses have been performed using a high-performance methodology that results in comparison measurement uncertainties that are significantly less than the uncertainties of the certified values of the calibration CRM. Consequently, the determined values have uncertainties that are very nearly equivalent to the uncertainties of the calibration CRM. Several uses of this calibration transfer are proposed, including, re-certification measurements of replacement CRMs, establishing traceability of one CRM to another, and demonstrating the equivalence of two CRMs. RM 8704, a river sediment, was analyzed using SRM 2704, Buffalo River Sediment, as the calibration standard. SRM 1632c, Trace Elements in Bituminous Coal, which is a replacement for SRM 1632b, was analyzed using SRM 1632b as the standard. SRM 1635, Trace Elements in Subbituminous Coal, was also analyzed using SRM 1632b as the standard.