Agilent 8800 串联四极杆 ICP-MS

Advanced technology products containing rare earth elements (REEs) continue to evolve at a rapid pace. Consequently, the use of REEs has extended from well-established applications such as glass polishing, to high-performance magnets, high-tech catalysts, electronics, glass, ceramics, and alloys. An alloy of the second most abundant REE, neodymium (Nd), with iron and boron (NIB) is an important material in the super permanent magnets that are used in vehicle components, computer data storage devices, MRI scanners, and loudspeakers. Nd is also used to make glass and safety glasses (didymium) used by glassblowers and welders. As REEs are increasingly used in high-tech products, control of any impurities is important. For example, the presence of other REEs as contaminants in a purified single-element REE material may affect the functionality of the final product, so impurities in the REE oxide raw material must be carefully controlled.

碘 129 ( 129 I) 是一种长寿命的放射性核素（半衰期 1570 万年），由核武器试验和核电站或乏核燃料处理厂泄露释放到环境中。ICP-MS 是一种灵敏快速的检测技术，测定环境中的 129 I 和同样有重要分析意义的 129 I/127 I 比值只需要进行少量的样品处理。但因为以下两方面的原因使这个应用富有挑战性：129 I会受到来自 氙 129（129 Xe，氩等离子体气中的杂质）的干扰；129 I 在样品中的浓度极低。 因此，高灵敏度和低背景是准确测定 129 I 浓度和 129 I/127 I 比值的关键。

本应用摘要描述了用于分离和测定甲基汞和乙基汞的方法，该方法基于高效液相色谱 (HPLC)/电感耦合等离子体质谱 (ICPMS) 联用系统。汞的化学形态不同毒性不同，因此将汞元素从烷基化形式分离出即可提供重要信息，了解样品的实际毒性。HPLC-ICP-MS 方法可用于分析水和土壤样品。该方法对于水中 MeHg、EtHg 和 Hg2+ 的检测限低于 10 ng/L，而对于土壤样品中的汞化合物，回收率在 80% 至 120% 之间。

由于清洁空气法修正案的第二部分增加了废水排放的内容，因此美国环境保护署（USEPA）需修订有关蒸气发电行业的废水指导方针。这些条例要求大多数燃煤工厂洗涤 S02，而实施结果便是产生大量的“烟气脱硫”废水。修订后的废水指 导纲要将适用于“以电力分配和销售为主、主要利用化石型燃料（煤、油或气） 或核燃料与使用汽水系统作为热动力媒介的热循环相结合的发电厂”。这就包 括了美国大多数的大规模发电厂。这些发电厂（尤其是燃煤发电厂）产生的废水可能含有数百个到数千 ppm 的钙、镁、锰、钠、硼、氯化物、硝酸盐和硫酸盐。在这种基体中测定低 ppb 级有毒金属（包括 As、Cd、Cr、Cu、Pb、Se、Tl、V 和 Zn）对于 ICP-MS 技术来说是一种挑战，因为存在较高浓度的可溶解固体和来自基体的多原子离子的潜在干扰问题。

铀 236 是一种可长期存在的放射性同位素，主要由天然存在的痕量同位素 235U （丰度 0.72%）通过热中子俘获形成。该过程导致 236U 相对于主同位素 238U 的天然丰度 (236U/238U) 处于 10-14 - 10-13 的范围内。236U 还可形成于核燃料或核武器的铀浓缩过程中，也是核反应堆中浓缩铀燃料消耗时产生的废弃物。乏核燃料中的 236U/238U 比值高达 10-3，而环境中的背景水平也随全球性沉降效应升高至 10-7 - 10-8。因此，236U/238U 同位素比可用作追踪浓缩铀燃料、乏核燃料和核废料 的意外泄漏，并考察核技术对环境及人类健康影响的一种灵敏的方法。所以，用于准确测定全球性沉降物的仪器必须能够对 < 10-9 水平的 236U/238U 同位素比进 行分析。使用安捷伦的第二代 ICP-MS/MS 即 Agilent 8900 串联四极杆 ICP-MS 进行分析，因为它具有高灵敏度和扩展的质量数范围，能够测定以氧化物 (UO+) 和二氧化物 (UO2+)反应子离子形式存在的铀。

Hydride gases, such as phosphine and arsine, are important contaminants in process chemicals used in both the petrochemical and semiconductor industries. For example, the presence of phosphine, arsine, hydrogen sulfide and carbonyl sulfide in polymer grade ethylene or propylene can have a deleterious effect on catalysts used in the production of polypropylene plastics. Accurate data on the concentrations of these contaminants at trace levels enables prediction of catalyst lifetime and minimizes production downtime.In the semiconductor industry, phosphine is used as a precursor for the deposition of group III-V compound semiconductors, and as a dopant in the manufacturing of semiconductor devices, such as diodes and transistors. In the case of group III-V compound materials, such as indium phosphide (InP), absence of other hydride dopant impurities e.g., silane, germane or hydrogen sulfide (and moisture) is critical, as they can have a profound effect on the performance of the final device. In particular, incorporated sulfur from hydrogen sulfide and carbonyl sulfide may affect the electrical properties of

Hydride gases, such as phosphine and arsine, are important contaminants in process chemicals used in both the petrochemical and semiconductor industries. For example, the presence of phosphine, arsine, hydrogen sulfide and carbonyl sulfide in polymer grade ethylene or propylene can have a deleterious effect on catalysts used in the production of polypropylene plastics. Accurate data on the concentrations of these contaminants at trace levels enables prediction of catalyst lifetime and minimizes production downtime.In the semiconductor industry, phosphine is used as a precursor for the deposition of group III-V compound semiconductors, and as a dopant in the manufacturing of semiconductor devices, such as diodes and transistors. In the case of group III-V compound materials, such as indium phosphide (InP), absence of other hydride dopant impurities e.g., silane, germane or hydrogen sulfide (and moisture) is critical, as they can have a profound effect on the performance of the final device. In particular, incorporated sulfur from hydrogen sulfide and carbonyl sulfide may affect the electrical properties of

Hydride gases, such as phosphine and arsine, are important contaminants in process chemicals used in both the petrochemical and semiconductor industries. For example, the presence of phosphine, arsine, hydrogen sulfide and carbonyl sulfide in polymer grade ethylene or propylene can have a deleterious effect on catalysts used in the production of polypropylene plastics. Accurate data on the concentrations of these contaminants at trace levels enables prediction of catalyst lifetime and minimizes production downtime.In the semiconductor industry, phosphine is used as a precursor for the deposition of group III-V compound semiconductors, and as a dopant in the manufacturing of semiconductor devices, such as diodes and transistors. In the case of group III-V compound materials, such as indium phosphide (InP), absence of other hydride dopant impurities e.g., silane, germane or hydrogen sulfide (and moisture) is critical, as they can have a profound effect on the performance of the final device. In particular, incorporated sulfur from hydrogen sulfide and carbonyl sulfide may affect the electrical properties of

LC-MS/MS is widely used in every stage of drug development, from discovery and characterization through manufacturing and quality control of the final pharmaceutical product. Due to its excellent selectivity for complex molecules, LC-MS/MS is an effective tool for both non-target qualitative analysis and quantitative analysis of targeted compounds. However, the sensitivity of LC-MS/MS varies significantly depending on the molecular structure of each compound, and can be affected by other coexisting substances in the sample. This limitation means that LC-MS/MS is often unable to provide accurate quantitative analysis without a compound-specific calibration standard. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a fast multi-element technique capable of accurate elemental quantification at trace and ultra-trace levels. While more widely adopted in inorganic, “metals” laboratories, ICP-MS is also used in the field of pharmaceutical analysis when a heteroatom-containing drug is the focus of interest [1, 2]. ICP-MS employs a high temperature plasma ion source that decomposes the sample to the atomic level. The high temperature

结合毛细管液相色谱分离技术，Agilent 8800 串联四极杆 ICP-MS 在 MS/MS 质量 转移模式下可痕量测定磷酸肽中的磷与含硫多肽中的硫。使用 LC-ICP-MS 可获得前所未有的含硫和含磷物质的最低绝对检测限（分别为 11 fmol 和 6.6 fmol）。 硫的同位素比值测定结果与其理论值高度吻合，从而证明干扰得以有效消除。 所观测到的硫和磷的峰形和信噪比表现优异。测定结果表明串联四极杆capLCICP-MS 技术在使用非特殊标样测定含硫和含磷多肽的高灵敏度和同时绝对定量分析方面有巨大潜力。

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used increasingly in metallomic studies to analyze metals and metal species and their interactions within biological and ecological systems. It is an elemental detection technique that uses a very high temperature argon plasma as the ion source. As a result, a given concentration of an element provides a signal that is broadly consistent, irrespective of the compound structure or sample matrix. Key to achieving accurate and reliable measurements is the ability to reduce and eliminate polyatomic interferences that otherwise would bias the analytical results. Recent development of a triple quadrupole ICP-MS (ICP-QQQ) dramatically improves the efficiency and reliability of removal of spectral interferences, making it easier to analyze elements with spectral overlaps such as iron, sulfur and selenium. Furthermore, the more effective removal of spectral overlaps allows access to multiple isotopes of many elements, enabling quantification of metalloproteins and peptides through the use of isotope dilution mass spectrometry (IDMS) analysis, which eliminates the requirement for compound specific calibration standards [1]. This absolute quantification technique allows accurate

食品中潜在有毒元素和化合物的存在日益受到公众的密切关注，因此，食品生产者及管理部门就要求有快速、可靠的筛选方法来准确定量食品和饮料中这些污染物的含量。对于砷 (As) 而言，它在食品中的富集浓度可能会通过以往含砷农药如砷酸氢铅（砷酸铅）或砷酸钙的使用而上升。这些化合物作为收获前农药在20 世纪广泛用于控制水果类作物（主要是苹果）上的害虫，如苹果蠹蛾、苹果蛆和果蝇。虽然在 1970 年禁止了这些农药的广泛使用，但是砷酸铅和砷酸钙非常稳定并可长期存留于土壤之中，因此在其应用被禁止很长时间以后仍可以影响在污染土壤中生长的作物。

Concern about the impact on public health from potentially toxic elements and compounds present in everyday foodstuff has led to new legislative guidance. The inorganic forms of arsenic (As) are known to be toxic and carcinogenic to humans, and food and drink are a potential source of exposure [1]. To reduce the intake of inorganic arsenic from the diet, the U.S. Food and Drug Administration (FDA) proposed a new action level for inorganic arsenic in apple juice of 10 μg/L in 2013 [2,3]. Also, following the eighth meeting of the CODEX Committee on Contaminants in Food, the World Health Organization (WHO) proposed a guideline for inorganic As in polished rice of 0.2 mg/kg [4]. There is a clear need for reliable screening methods to accurately determine the levels of such contaminants in food and drink products. The detection limits required are low, as a 0.2 mg/kg limit equates to a digestate concentration of 2 μg/L (assuming a 100x digestion dilution). Even small errors in the precision and accuracy of the analytical method could result in a food product being wrongly classified as safe. Selenium (Se) is an essential micronutrient that can be deficient in the diet as Se-poor soils yield Se-poor food crops. Accurate quantification of Se in food is necessary to assess nutrient status.

The determination of pesticide residues in food products is important especially for infants and children, as the quantity of food they ingest per kilogram of body weight is relatively high. Some pesticides are known or suspected endocrine disrupting chemicals (EDCs), so the potential for interference with the function of the naturally occurring hormones can severely impact a growing child, even at low concentrations. The implications of long-term, low-dose exposure through food consumption have led to interest in development of highly sensitive analytical methods that combine rapid sample preparation with hyphenated separation and detection. Most pesticide residue laboratories use some variation of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction methods. Often the extracted material is analyzed using gas chromatography-tandem mass spectrometry (GC/MS/MS) for the thermally stable, less polar pesticides, or liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for the less volatile and/or more polar ones. A more recently developed alternative technique involves coupling GC to triple quadrupole ICP-MS (GC-ICP-QQQ), which is able to Determination of pesticides in foods using phosphorus and sulfur detection by GC-ICP-QQQ Application note Authors Jenny Nelson1-3, Helene Hopfer1-2,4, Fabio Silva3 , Steve Wilbur3 , Jianmin Chen3 , Kumi Shiota Ozawa3 and Philip L. Wylie5 1 Department of Viticulture and Enology, University of CaliforniaDavis, Davis CA, USA 2 Food Safety and Measurement Facility, University of CaliforniaDavis, Davis CA, USA 3 Agilent Technologies, Inc., Santa Clara CA, USA 4 HM Clause, Davis CA, USA 5 Agilent Technologies, Inc., Wilmington DE, USA Food testing 2 determine pesticides by measuring the heteroatoms P and S (also Cl and Br) contained in most pesticides. GC-ICP-QQQ offers very good selectivity and specificity, and sensitivity that can be greater than the established methods. The method described in this work ca

Concern about the impact on public health from potentially toxic elements and compounds present in everyday foodstuff has led to new legislative guidance. The inorganic forms of arsenic (As) are known to be toxic and carcinogenic to humans, and food and drink are a potential source of exposure [1]. To reduce the intake of inorganic arsenic from the diet, the U.S. Food and Drug Administration (FDA) proposed a new action level for inorganic arsenic in apple juice of 10 μg/L in 2013 [2,3]. Also, following the eighth meeting of the CODEX Committee on Contaminants in Food, the World Health Organization (WHO) proposed a guideline for inorganic As in polished rice of 0.2 mg/kg [4]. There is a clear need for reliable screening methods to accurately determine the levels of such contaminants in food and drink products. The detection limits required are low, as a 0.2 mg/kg limit equates to a digestate concentration of 2 μg/L (assuming a 100x digestion dilution). Even small errors in the precision and accuracy of the analytical method could result in a food product being wrongly classified as safe. Selenium (Se) is an essential micronutrient that can be deficient in the diet as Se-poor soils yield Se-poor food crops. Accurate quantification of Se in food is necessary to assess nutrient status.

A fast and sensitive method using hydride generation (HG) with ICP-MS has been developed for the separation and detection of inorganic arsenic (iAs) in foodstuffs. The iAs measured values in 31 commercial rice products all fell below the current legislative maximum level (ML) of 150 μg/kg set by China. Comparing the results obtained by HG-ICP-MS and HPLC-ICP-MS showed comparable limits of detection were achieved. HG-ICP-MS is ideally suited to the large scale screening of food samples, such as rice, as analysis can be performed in a fraction of the time typically required by a conventional HPLC-ICP-MS approach, with no compromise in analytical performance.

一些金属对人体来说不可或缺，而另一些则含有剧毒。因此，在食品生产的每一个阶段都需要监测痕量金属元素。 借助安捷伦的原子光谱产品系列产品 – AA、MP-AES、ICP-OES、ICP-MS（包括 ICP-MS/MS）和 HPLC-ICP-MS，能够快速筛查食品和饮料。 1，快速筛查有毒和有益的金属元素 2，分析大量元素和食品类型 3，测定痕量、微量及常量元素的浓度

在半导体工业，严格控制半导体器件生产过程中所使用化学品中的金属杂质，对于实现所需的产品性能和产量至关重要。随着半导体器件性能的持续提高，对杂质的控制要求也更加严格。例如，生产过程中所使用超纯水 (UPW) 中的金属含量必须控制在亚 ppt 水平。ICP-MS 是半导体工艺化学品和器件中痕量金属分析的标准技术。半导体工业中最常用的仪器和测试技术是带冷等离子体的单四极杆 ICP-MS (ICP-QMS)。开发于上世纪 90 年代中期的冷等离子体技术，可定量分析 ppt 水平主要污染物元素。从 2000 年开始建立起来的带碰撞反应池的 ICP-QMS，可以实现更复杂半导体基质的直接分析，但是不能改善冷等离子体的检测限或背景等效浓度 (BEC)。为实现亚 ppt 水平的检测，要求必须降低BEC。 Agilent 8800 电感耦合等离子体串联质谱仪 (ICP-MS/MS)采用新型反应池技术，对于 Ca 的分析可得到 100 ppq 的背景等效浓度 (BEC)。本文描述了采用 Agilent 8800 ICPMS/MS 分析超纯水中亚 ppt 水平 Ca 的原理和操作。