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A Study of Matrix Effects on Multiply Charged CompoundsIn preclinical development, the absolute quantification of peptides in biological matrices becomes a challenge due to the limited availability of stable label internal standards and affinity-based cleanup. This puts a renewed emphasis on matrix effects, especially for the bioanalysis of hydrophobic peptides. While the impact of matrix effects has been studied for extensively singly charged small molecules, their effect on multiply charged compounds has yet to be characterized fully. This article discusses initial results from matrix effect experiments in relation to the bioanalysis of hydrophobic peptides and techniques used to minimize matrix effects.
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The Impact of Illegal Artisanal Gold Mining on the Peruvian Amazon: Benefits of Taking a Direct Mercury Analyzer into the Rain Forest to Monitor Mercury ContaminationIllegal artisanal gold mining using mercury amalgamation is poisoning people and the ecosystem in the Amazon rain forest. By taking the technique of direct mercury analysis to a remote, field-based laboratory, the team of Professor Luis Fernandez is measuring the extent of the contamination in a wide variety of samples, including soil, fish, air and human hair.
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Liquid Chromatography–Time-of-Flight Mass Spectrometry for Cannabinoid Profiling and Quantitation in Hemp Oil ExtractsThe method presented here allows for the accurate, precise, and robust speciation, profiling, and quantification of cannabinoids in hemp oil extracts and commercial cannabinoid products for research and development laboratories.
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Confocal Raman AFM Imaging of PaperA better understanding of the micro- and nanostructures of cellulose fiber composition before and after various chemical treatments, together with the distribution of bleaching additives to the final paper composition, is essential for further improvements of paper properties. Confocal Raman imaging is a valuable tool for such studies, as it reveals not only optical information but also information regarding the 3D distribution of the chemical compounds in the submicrometer range. In the paper surface finishing process, additional surface roughness parameters can be measured by combining confocal Raman microscopy with atomic force microscopy. Such combined analytical microscopes allow a direct linking between high-resolution imaging and chemical identification of various species on a surface.
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Qualitative and Quantitative Metabolite Identification for Verapamil in Rat Plasma by Sub-2-μm LC Coupled with Quadrupole TOF-MSAn effective metabolite identification study should ideally include both qualitative and quantitative information that for both identifying metabolites, and determining the rate of clearance and the metabolic routes of the parent drug. Liquid chromatography–mass spectrometry (LC–MS) is considered the standard analytical technique for metabolite identification studies. To date, however, qualitative and quantitative information has always been obtained from two separation platforms: quadrupole time-of-flight (QTof) MS for the exact mass full-scan qualitative study, and tandem quadrupole MS for the multiple reaction monitoring (MRM) quantitative study. With advancements to QTof instrumentation, specifically, recent improvements in sensitivity and dynamic range, it is now possible to perform both qualitative and quantitative experiments on a single QTof mass spectrometer. This article describes a workflow that allows simultaneous qualitative and quantitative metabolite identification studies to be..
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Quantitative Proteomic Workflow for Discovery of Early Rejection Kidney Transplant Peptide Biomarkers and Subsequent Development of SRM Assays in UrineThe authors discuss a noninvasive method for determining early indications of the rejection of a kidney transplant.
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Detection and Sourcing of Counterfeit Pharmaceutical Products and Consumer GoodsThe authors discuss the use of vibrational spectroscopy to differentiate an authentic article from a counterfeit one throughout a product's lifecycle, from component receipt at the site of manufacture, to product receipt by the end user.
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Comparison of Secondary Structures of Similar Proteins Using Automated CDIn this study, far-UV CD spectra of eight different mammalian serum albumins were measured repeatedly using automated CD spectroscopy. Two independent methods of normalizing the CD data were used to eliminate the need for accurate knowledge of protein concentration or extinction coefficient. The normalized far-UV data, representative of secondary structure, were compared to determine if there were statistically significant differences between samples. The two normalization methods agreed in every case, increasing confidence in the results.
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Analysis of the State of the Art: Infrared SpectroscopyIn honor of Spectroscopy's celebration of 30 years covering the latest developments in materials analysis, we asked a panel of experts to assess the current state of the art of infrared (IR) spectroscopy and to try to predict how the technology will develop in the future.
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Finding Gold Just Became Easier than Ever ImaginedPhotonic Knowledge, Inc., a spin-off of Photon etc., introduces the Core Mapper?, a hyperspectral imager that produces instantaneous, precise in situ mineralogy, lithology, and alteration mapping. This unique patented technology answers the increasing demand of the mining industry for better exploration tools.
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Dried Blood Spots and High-Resolution Mass Spectrometry for Discovery Fast PK BioanalysisThis article introduces the advantages of accurate mass high-resolution mass spectrometry LC–MS (HRMS) coupled to the dried blood spot (DBS) technique for fast PK applications in a discovery environment. Compared with the established norm of plasma bioanalysis using triple quadrupoles, HRMS coupled to DBS is a viable alternative. The benefit is access to critical new information (HRMS bioanalysis) and significantly less stress on the animal (DBS), both factors that potentially improve the quality of early PK data.
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Advances in TOF-MS-Based Screening for Food Safety Residue Analysis with a Positive ApproachMass spectrometry plays an increasingly significant role in the analysis of residues and contaminants in food. Here we will illustrate how the combination of ultrahigh-pressure liquid chromatography (UHPLC) and high-resolution time-of-flight-mass spectrometry (TOF-MS) is used to generate a screen of veterinary drug residues in products of animal origin. The use of UHPLC–TOF-MS and dedicated, workflow directed software allows rapid screening for large numbers of residues and automated quantification of positive samples. In addition, we illustrate how the data generated using MSE acquisition mode enable critical structural information to be collected, which offers additional selectivity and confirmatory data for compound identification and facilitates elucidation of the structure of newly discovered compounds.
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Raman Spectroscopy of DocumentsDocuments have been investigated to determine the feasibility of utilizing Raman and SERS Raman spectroscopy for the identification and characterization of inks on paper. Fluorescence reduction methods have been employed to facilitate the analysis by reducing the nascent fluorescence from paper and ink. Furthermore, ink crossings were investigated to demonstrate that ink applied after creation of a document could be differentiated from the originally applied ink.
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Monitoring Polymer Phase Transitions by Combining Rheology and Raman SpectroscopyThe in situ combination of rheometry and Raman spectroscopy allows for real-time, synchronized measurement of both physical and chemical material properties.
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IC–ICP–MS Speciation Analysis of As in Apple JuiceIn this study, apple juice samples are analyzed by IC–ICP–MS to determine the concentration of six arsenic species: the two inorganic, and highly toxic, species (As (V) and As [III]) and four organic species (arsenobetaine [AsB], arsenocholine [AsC], monomethylarsonic acid [MMA], and dimethylarsinic acid [DMA]).
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Enhancing the Sensitivity of Atmospheric Pressure Ionization Mass Spectrometry Using Flow Modulated Gas ChromatographyThe past decade has witnessed resurgent interest in coupling GC to atmospheric-pressure chemical ionization (APCI), which is suitable for the high column flows required for using flow modulation. This study assesses the use of GP-APCI with flow modulation for sensitive detection of selected trace organics.
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The Orbis Micro-XRF Analyzer SeriesBuilding on more than 10 years of Micro-XRF experience, the Orbis spectrometer yields a system with excellent Micro-XRF capability while setting a new standard in analytical flexibility. The Orbis incorporates a unique motorized turret integrating video and X-ray optics allowing coaxial sample view and X-ray analysis. The turret can accommodate two additional collimators along with the X-ray optic for a total of three X-ray beam sizes to expand the Orbis analytical capabilities beyond traditional Micro-XRF analysis.
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Metabolite Profiling Applications in Early Drug DiscoveryMetabolite profiling in drug discovery can contribute significantly at the lead optimization stage in two main application areas. The first is the identification of major metabolites, which provides medicinal chemists with information on the metabolic "soft spots." These soft spots are locations on the molecule particularly susceptible to metabolic modification, which can contribute to high pharmacokinetic clearance. This information then can be used to optimize the structure of a lead compound or chemical series to slow the rate of metabolism and therefore reduce hepatic clearance. This improves the absorption, distribution, metabolism, and excretion (ADME) properties of the compound, such as bioavailability, exposure (as measured by area under the curve), and half-life. Through iterative optimization of the structure and timely generation of metabolism data following each structural modification, pharmacokinetic properties can be improved while maintaining activity against the therapeutic target.
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Raman Analysis of Embedded ContaminantsRaman confocal spectroscopy is increasingly being applied for the analysis of embedded contaminants within materials. A non-contact, non-destructive analysis method, Raman spectroscopy requires very little sample preparation, has greater spatial resolution compared to FT-IR microscopy and the confocal analysis method allows visualization of materials within a clear sample matrix. This paper will investigate the analysis of an embedded contaminant within a polymer matrix on a glass substrate.
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Atomic Absorption: Feeding the Food Safety MarketWhile viewed as a mature technology, atomic absorption is still an attractive choice, particularly in the area of food safety.
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The Determination of Selenium in Shampoo by Flame Atomic Absorption SpectrometryThe formal European Union analytical method to measure and regulate the concentration of selenium disulphide is by the determination of selenium via flame atomic absorption spectrometry.
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Review of New Spectroscopic Instrumentation for 2018Our annual review of spectroscopy products, broken down into the following categories: Atomic Spectroscopy, Florescence, Mass Spectrometry, Mid-IR, NIR, NMR and ESR, Raman, UV-vis, X-ray, Software, Accessories, Components
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Online Identification of Flavones from Flos Chrysanthemi by LC–MS-IT-TOFThe use of medicinal herbs as alternative treatment methods continues to grow. With this escalating use has come an increasing interest in determining the chemical compositions of these herbs in order to obtain a better understanding of their makeup and effects. In this study, Flos Chrysanthemi, a commonly used traditional Chinese medicine that has been cultivated for centuries, was analyzed to identify the main flavone compositions in one original breed of Flos Chrysanthemi (Hangbaiju) in China.
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Meeting the Surge in Demand for Seafood Screening on the Gulf CoastThe authors look at the use of QuEChERS in the ongoing testing program in the gulf.
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Advances in TOF-MS-Based Screening for Food Safety Residue Analysis with a Positive ApproachMass spectrometry plays an increasingly significant role in the analysis of residues and contaminants in food. Here we will illustrate how the combination of ultrahigh-pressure liquid chromatography (UHPLC) and high-resolution time-of-flight-mass spectrometry (TOF-MS) is used to generate a screen of veterinary drug residues in products of animal origin. The use of UHPLC–TOF-MS and dedicated, workflow directed software allows rapid screening for large numbers of residues and automated quantification of positive samples. In addition, we illustrate how the data generated using MSE acquisition mode enable critical structural information to be collected, which offers additional selectivity and confirmatory data for compound identification and facilitates elucidation of the structure of newly discovered compounds.
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Using LC–oa-TOF MSE with a Multivariate Statistical Sample Statistical Sample Profiling Strategy to Distinguish Chinese Red Ginseng from Korean Red GinsengBoth Chinese ginseng and Korean ginseng are similar plant species and undergo similar handling procedures when harvested and processed for sale. Despite their similarities, Korean ginseng commands a higher price than Chinese ginseng on the open market and is believed to produce different clinical effects than Chinese ginseng. Chinese researchers are now employing new techniques on the two varieties of ginseng to understand their chemical differences. HPLC/UV-based strategies for distinguishing the two types of ginseng have proven to be mostly ineffective due to lack of resolution. Using UltraPerformance liquid chromatography/orthogonal acceleration (oa)–TOF mass spectrometry and exact mass measurement, the authors developed a high-resolution method using multivariate statistical analysis for separating and identifying differences between Chinese ginseng and Korean ginseng at the molecular level.
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Ultratrace Aluminum Analysis of Nutritional Intravenous Solution Components in 1-Propanol Using GFAAS (PDF)This article describes how ultratrace aluminum analysis of two nutritional intravenous solution components with limited water solubility can be performed by graphite furnace atomic absorption spectroscopy (GFAAS) with dissolution in 1-propanol.
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Why and How to Avoid Ionic Contamination in Water Used for LC–MS AnalysesIonic contaminants in the water used in UHPLC analyses with MS detection method lead to adduct formation and reduced analytical signals because of ion suppression. In MS, the preferred ion type is the protonated molecular ion, especially in peptide analysis, since the partially mobile proton charge enables more meaningful fragmentation analysis, as compared to a sodiated peptide ion.
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Spectroscopic Monitoring of the Enrichment of Chlorin e6 in Tumors of the SkinFor the optimization of photodynamic therapy the spectroscopic detection of photosensitizer molecules, which are selectively enriched in tumour cells, can be useful.
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Using LC–oa-TOF MSE with a Multivariate Statistical Sample Statistical Sample Profiling Strategy to Distinguish Chinese Red Ginseng from Korean Red GinsengBoth Chinese ginseng and Korean ginseng are similar plant species and undergo similar handling procedures when harvested and processed for sale. Despite their similarities, Korean ginseng commands a higher price than Chinese ginseng on the open market and is believed to produce different clinical effects than Chinese ginseng. Chinese researchers are now employing new techniques on the two varieties of ginseng to understand their chemical differences. HPLC/UV-based strategies for distinguishing the two types of ginseng have proven to be mostly ineffective due to lack of resolution. Using UltraPerformance liquid chromatography/orthogonal acceleration (oa)–TOF mass spectrometry and exact mass measurement, the authors developed a high-resolution method using multivariate statistical analysis for separating and identifying differences between Chinese ginseng and Korean ginseng at the molecular level.
