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Implementation of Methods Translation between Liquid Chromatography InstrumentationPharmaceutical research and development (R&D) organizations were early adopters who recognized the many benefits of UltraPerformance LC? (UPLC?) Technology including resolution, sensitivity, throughput, and productivity as compared to HPLC.
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Nonconventional Alternatives to LC–MSAn important attribute of a novel ionization process for use in mass spectrometry (MS) is its simplicity and flexibility to be hyphenated to conventional liquid-based separation methods.
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Standardized Testing of Silica as a Base Material for Difficult Bonded-Phase Preparative ApplicationsThis year's symposium was held in New Orleans, Louisiana, USA. In this review, Ron Majors covers HPLC and UHPLC column and sample preparation highlights, summarizes the awards presented, and reviews the overall liquid-phase chromatographic trends.
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New Method US EPA 625 with Solid Phase Extraction for Challenging WastewatersThis automated SPE methodology is a solution that will reduce analyst labor, solvent usage, and turn-around-time while maintaining the high quality results required within today's laboratories.
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Flow-Modulated Comprehensive 2D Gas Chromatography–Triple Quadrupole MS Elucidation of the Fatty Acids and Unsaponifiable Constituents of Oil Derived from Lemon Seeds, A Food-Industry Waste ProductThis article is focused on the detailed qualitative analysis of the fatty acids and the unsaponifiable constituents of a vegetable oil derived from a food-industry waste product, namely lemon seeds.
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Combining Different Stationary-Phase Chemistries to Improve the Selectivity of Impurity Profiling MethodsSerial coupling of different column types can provide several important benefits to the chromatographer, including fine-tuning selectivity to separate complex mixtures.
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The Preparative Use of Flow Field-Flow FractionationDemonstrating that flow field-flow fractionation can separate protein aggregates for preparative and analytical purposes.
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Extraction of Cannabinoids from BrowniesCannabinoids are successfully extracted from a complex brownie matrix using the QuEChERS sample preparation technique, significantly reducing the presence of matrix interferences. The resulting clean samples are analyzed by GC–MS using a specialized deactivated GC column to provide heightened peaks for the cannabinoid compounds.
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Inaccuracies in the Quantification of Peptides — A Case Study Using β-Endorphin AssayThis article describes possible sources of error that may contribute to significant inaccuracy in peptide assay methods: The fi ltration material (cellulose) used in sample clean up and the vial material (glass and plastic) used in LC analysis. This study is based on ?-endorphin but has relevance for most peptide assays.
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Direct Analysis of Drugs in BiofluidsSample pretreatment is often a time consuming and labor-intensive step which can be a restricting factor for the rapid analysis. This is especially true for the analysis of drugs in biofluids containing many interfering matrices.
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A Convenient Alternative to MALDI and ESIIonization of small, large, volatile, and nonvolatile compounds with charge states nearly identical to electrospray ionization are produced from a solid matrix or solution with high sensitivity utilizing the vacuum inherent with any mass spectrometer. With the proper matrix, analytes can be analyzed from ambient conditions or by direct introduction into vacuum.
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Consolidated GC-MS/MS Analysis of OCPs, PAHs, and PCBs in Environmental SamplesAnalysis of OCPs, PAHs and PCBs in environmental samples through a consolidated GC-MS/MS method using the Thermo Scientific™ TRACE™ 1310 GC and the TSQ™ 8000 triple quadrupole GC-MS/MS.
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LC/LC–MSA snapshot of key trends and developments in the chromatography sector according to selected panelists from companies exhibiting at Analytica 2018.
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SFC–GCxGC to Analyse Matrices from Petroleum and CoalSFC–GCxGC is shown to be useful in fossil fuel analysis. Practical examples for the analysis of complex matrices are described.
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Determination of α-Amanitin in Human Serum by Solid-Phase Extracton Coupled with HPLC-UVA method is presented for the determination of ?-amanitin, a toxic cyclic octapeptide of amanitin mushrooms, in human serum by solid-phase extraction coupled with high performance liquid chromatography with UV detection.
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Direct Analysis of Drugs in BiofluidsSample pretreatment is often a time consuming and labor-intensive step which can be a restricting factor for the rapid analysis. This is especially true for the analysis of drugs in biofluids containing many interfering matrices.
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Lab Coping Helium ShortageNote discusses how labs are coping with the worldwide helium shortage.
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Quantitative Comparison of Hormones in Drinking Water Between Low and High Resolution Mass SpectrometryThe quantitative performance of the latest generation of high-resolution instruments is comparable to that of a triple quadrupole MS, even though different scanning modes are used. Higher-resolution instrumentation also allows flexibility concerning compound identification because the experiment can be set up for targeted quantitation, screening, or both. In an Orbitrap-based instrument, the parallel reaction monitoring (PRM) mode performs most closely to a triple quadrupole mass analyzer using selected reaction monitoring (SRM) mode. This study looks at the performance of an Orbitrap-based LC–MS method for EPA Method 539.
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Chiral Purification with Stacked Injections and Collections Using the Prep 100 SFC MS Directed SystemChiral chromatography has become the preferred tool for enantiomer separations in the early stages of pharmaceutical development for the purpose of accurately identifying single pure enantiomers with pharmacologic, toxicological, and clinical information, as stipulated by the FDA.1
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A QbD with Design-of-Experiments Approach to the Development of a Chromatographic Method for the Separation of Impurities in VancomycinAnalytical methods are developed at various stages of the drug develoment process for samples of varying complexity.
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Torun Triumph: ISC 2012 ReviewProfessor Boguslaw Buszewski, Chairman of ISC 2012 and President of EuSSS, CeGSS and the Polish Chemical Society, reveals the highlights of last year's illuminating programme.
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Validation of LC–MS-MS Methods for the Determination of Ibuprofen in Miniature Swine Plasma and Synovial FluidPublished methods for the determination of ibuprofen in biological fluids by liquid chromatography (LC)–UV or LC–mass spectrometry (MS)-MS have quantitation ranges consistent with the relatively high but typical ibuprofen dose (200–800 mg), generally having lower limits of quantitation in the low micrograms-per-milliliter range. For the analysis of plasma and synovial fluid samples from preclinical (miniature swine) studies utilizing a novel ibuprofen dosage form, LC–MS-MS methods were developed and validated over the 10–1000 ng/mL range. Ibuprofen undergoes biotransformation to ibuprofen acyl glucuronide and sublimes under routine bioanalytical sample handling conditions. Procedures were implemented to minimize the impact of these potential liabilities.
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Choosing an Optimal Co-Solvent for Method Development in Supercritical Fluid Chromatography (SFC) for the Whelk-O®1, RegisPack®, and RegisCell® Chiral Stationary PhasesThe majority of the samples in this study and other studies show that a majority of compounds can be separated by the use of the three most common alcohols: IPA, CH3OH, and ethanol. Solubility becomes a crucial factor in preparative chromatography. Combinations of solvents can be used to improve solubility when the chosen co-solvent has poor solubility of the compound in question.
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Simplifying Mass Spectrometry Through New Ionization Technology: Application to Drugs and Clinical AnalysesA newly discovered method, matrix-assisted ionization (MAI), is described for generating gas-phase ions from volatile and nonvolatile compounds. The method is both simple and sensitive.
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Development and Validation of an HPTLC Method for Determination of Aflatoxin B1A high performance thin-layer chromatographic (HPTLC) method was developed for the determination of aflatoxin B1 in cereals.
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Identifying "Known Unknowns" in Commercial Products by Mass SpectrometryThe identification of nontargeted species in environmental and commercial samples by mass spectrometry can be very difficult. In this article, authors from Eastman Chemical Company describe their systematic approach for the identification of nontargeted species using nominal and accurate mass data, searching both mass spectral and "spectra-less" databases.
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Application of Paper Strip Extraction in Combination with LC–MS-MS in PharmacokineticsRecent advances in sampling techniques in the pharmaceutical industry sparked significant interest in applying improvements to extraction methods for greater analyte detection and quantitation.
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Improving the Universal Response of Nebulization-Based UHPLC DetectionHigh performance liquid chromatography (HPLC) with light absorbance detection (UV) is limited by the dependence of detector response on the structure of the analyte. Some detection techniques based on nebulization of the mobile phase and formation of Aerosol particles demonstrate an analyte independent response that approaches "universal."
