ICP-MS

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The ability to perform accurate mass measurements in mass spectrometry (MS) for elemental composition determination (ECD, also known as formula identification) provides a powerful tool for assisting in the identification of unknown compounds. Recent advances in data processing methods have demonstrated the ability to obtain mass accuracy in the 5–10 ppm range on routine single- and tandem-quadrupole systems (1,2), sufficient to assist in the formula identification. However, even on more expensive high-resolution systems such as quadrupole time-of-flight (qTOF) or Fourier transform (FT)–MS instruments that are capable of routinely measuring mass accuracy in the 1–3 ppm range, the formula identification is not unique, particularly for higher molecular weight compounds. By calibrating instruments to obtain high spectral accuracy as well as mass accuracy, the ability to unambiguously identify the formula is improved substantially, particularly on low-resolution systems.

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Gas chromatography–mass spectrometry (GC–MS) and liquid chromatography (LC)–MS are widespread successful approaches, based on single-quadrupole MS, for the routine detection, identification, and quantitation of compounds. There has, however, been increasing interest in the use of tandem MS in more challenging, complex matrices such as those commonly found in food, environmental, and biological analyses. The combination of GC with tandem-quadrupole MS (MS-MS) is discussed, where the inherent increase in selectivity and sensitivity of the approach has enabled rapid, confident compound detection and quantitation for such demanding applications.

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The 30-year history of advances in gas chromatography–mass spectrometry technology continues today. Recent improvements in hardware, electronics, and data analysis software have resulted in new levels of productivity and sensitivity that have broadened the potential applications for this laboratory mainstay.

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Mass spectrometers are effective for identifying and quantifying unknown molecules, such as disease-related proteins and small molecules in pharmaceutical research and medical diagnosis. In addition, mass spectrometry (MS) can be particularly powerful when analyzing molecules with complex structures, such as posttranslationally modified proteins. Among various MS approaches, high-resolution multistep tandem MS (MS-MS) is an emerging methodology for accurate identification of complex molecules. In this article, we describe a new approach for mass analysis with enhanced quantitative capability combined with high-resolution multistep MS-MS, where the dynamic range of quantitation covers four orders of magnitude.

January 2007. Because of concerns over increasing levels of anthropogenic pollutants in the Great Salt Lake in Utah, the Utah Division of Water Quality recently conducted a roundrobin study of selenium in ambient and spiked Great Salt Lake waters to determine the most practical analytical technique for its detection. Of the techniques applied, only hydride generation atomic absorption and octopole reaction system ICP-MS provided acceptable results.

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Mass spectrometry has long been a preferred tool for protein identification and biomarker discovery, but preparation of biological samples remains a challenge. Hindrances include the wide range of protein concentrations, sample complexity, and loss or alteration of important proteins due to sample handling. This article describes recent developments in sample fractionation technologies that are overcoming these challenges in interesting ways and are enabling in-depth proteomic studies that were not possible in the past.

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Serum protein profiling using mass spectrometry (MS) is one of the most promising approaches for biomarker identification. The authors adopted a nano liquid chromatography (nLC)–linear ion trap time-of-flight (LIT-TOF) MS system and newly developed software known as information-based acquisition (IBA) to identify biomarkers in human serum. IBA is a data processing protocol for repetitive MS analyses. Peptides selected for the first-pass MS-MS analysis are automatically excluded from the MS spectrum such that subsequent MS-MS analyses are performed on different peptides to minimize overlapping analyses, resulting in the identification of relatively low-abundant peptides.

Enabling targeted quantitative proteomics applications and hypothesis-driven inquiries will help researchers to understand how proteins function in living systems. The discovery and validation of small molecule and protein-based biomarkers, and the eventual translation of these discoveries from the research lab to the clinic, involves robust mass spectrometry (MS) systems and software that make it easier for technicians to perform routine sample analyses on liquid chromatography (LC)–MS-MS systems, which continue to be used in an increasing number of both protein and small molecule analysis applications.

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Ultrahigh performance liquid chromatography (LC)–time-of-flight mass spectrometry –(TOF-MS) and gas chromatography (GC)–TOF-MS are powerful approaches for screening target compounds and identifying or characterizing nontarget compounds in complex mixtures. The combination of accurate mass data and newly developed software enables truly generic screening methods with TOF-MS, and the confident detection, identification, and confirmation of small molecules in a range of application areas.

Accurate determination of trace Cl, Br, and I is important in industries such as petrochemical refining, chemical manufacturing, biomedical and nutritional supplement manufacturing, and environmental analysis. Until recently, it was thought that the halogen elements could not be determined effectively by inductively coupled plasma–optical emission spectroscopy (ICP-OES); however, with recent advances in spectrometer and detector design, these elements are now readily determined. In fact, ICP-OES offers many advantages for the measurement of Cl, Br, and I. These include ease-of-use and the ability to test for other elements simultaneously, along with good sensitivity, precision, and accuracy. This article describes the measurement of chlorine in tissue and oil samples as well as the measurement of bromine in plastics and electronic materials where the solids were sampled using laser ablation.

Interactive dedicated tools have been developed to facilitate the use of multiline analysis in inductively coupled plasma–atomic emission spectroscopy (ICP-AES) with emphases on multiline selection and on statistics for rejection of possible outliers. The aim is to take full benefit of the available information when using a charge-coupled device (CCD) detector–based instrument and to enhance the accuracy of the results. Determination of Cu in steel will be used to illustrate the potential of the tools.

The use of fertilizers is important to increase crop yields in soils that are being used for agricultural purposes. However, in order to maximize plant growth, it is also absolutely essential to know how the crops are using the nutrients in the soil. This process is commonly referred to as a fertility management program, where many soil samples are taken over a predefined area of the land and analyzed for various components such as pH, organic matter, and trace element nutrients. This article describes how a soil testing laboratory in the midwest has developed a method to analyze up to 3500 soil samples per day for 11 trace metals, using inductively coupled plasma–optical emission spectroscopy. It will focus on the soil sampling procedure together with the sample preparation requirements for this high workload environment. The instrumental analytical procedure will be described in greater detail, particularly how the measurement protocol and sampling process are optimized to cope with such extreme..

The analysis of edible oils and fats by inductively coupled plasma–optical emission spectroscopy (ICP-OES) utilizing direct injection after dilution with kerosene is described. Sample preparation was performed according to EN ISO 661 (1) and ISO 10540-3 (2). The accuracy was investigated using the AOCS reference sample, "Trace Metals in Soybean Oil" (3) and by spike recovery measurements using commercial sunflower oil. The analysis requirements for sensitivity, precision, and accuracy were met. This article includes line selection, detection limits, and accuracy studies.

Although inductively coupled plasma–mass spectrometry (ICP-MS) has rapidly attained acceptance as the choice in trace metal analysis, most commercially available instruments are equipped with quadrupole-based mass analyzers. Quadrupole mass spectrometers have been available commercially for ICP since the early 1980s. Modifications and advances in these types of instruments predominantly have been in the sample introduction and ion optic areas, leaving the quadrupole mass spectrometer untouched.

Fertilizers are used to provide major plant nutrients (N, P, and K), secondary plant nutrients (Ca, S, and Mg), and micronutrients such as B, Mn, Fe, Cu, Zn, Mo, and Se. Accurate determination of the composition of fertilizers is essential so that the correct dose can be applied to the soil. An insufficient application of a fertilizer can result in poor crop yield, and an excessive application can result in environmental damage such as eutrophication by dissolved phosphates and nitrates entering water courses or land contamination from nonnutrient elements within the fertilizers. Inductively coupled plasma (ICP) spectroscopy offers cost-effective analysis of fertilizers because of its multielement capabilities. Complex torch designs and sparging systems have been employed in the past to determine nitrogen by ICP spectroscopy, but these additions to ICP instrumentation are costly and prolong analysis time.

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Elemental analysis in biological samples generally is achieved using flame atomic absorption spectrometry (AAS) and graphite furnace AAS (GFAAS). Flame AAS is fast, easy-to-use, and economical, but insufficiently sensitive for assays such as Se in serum and Pb/Cd in whole blood. These measurements require use of the more sensitive GFAAS. Inductively coupled plasma-mass spectrometry (ICP-MS), despite its low detection limit capabilities and wide elemental range, has had relatively little impact to date on biomedical analysis because of the popularly held conception that it is complex to use and expensive. In recent years, the instrumentation has been simplified and purchase, running, and maintenance costs have fallen. As a result, clinicians are becoming more interested in ICP-MS, although the perception that it is still much more expensive than GFAAS remains. This article provides a comparison of the costs of ICP-MS and GFAAS for biomedical sample analysis and illustrates the performance of ICP-MS for..

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Plutonium is distributed globally in the Earth's surface environment as a result of atmospheric weapons tests, nuclear accidents, and nuclear fuel reprocessing. Mass spectrometry (MS), in particular, sector field ICP-MS, now is used widely to determine Pu activities and isotope ratios; 240Pu/239 is very useful in determining Pu origin. Determination of Pu by ICP-MS involves dissolution, column separation, and the MS determination; detection limits are 0.1–10 fg for each isotope. Applications of the determination of sector field ICP-MS to studies of environmental Pu include discerning sources of contamination near the Chernobyl reactor, and chronology of recent aquatic sediments.