Pharmaceutique

Articles

8-Minute GC Analysis of Residual Solvents

Single-injection, dual-column detection/confirmation assay is feasible for regulated solvents in pharmaceutical products, but no temperature program provides sufficient resolution on both columns. Using a Restek G43/G16 column pair and independent temperature programs in a Gerstel MACH column heating system, we analyzed and confirmed 23 Class 2 solvents in 8 minutes.

Assaying Local Anesthetics by GC/FID

An Rxi®-5ms column and a wool-packed inlet liner provide the stability and inertness needed for these basic, active analytes. Chromatography from a six-replicate system suitability analysis was well within normal acceptance criteria. USP tailing factors were approximately 1.00 for all analytes; retention times and area responses were very stable.

Characterizing Cellular Fatty Acid Methyl Ester (FAME) Profiles to Identify Bacteria Using Gas Chromatography

Dr. Radomír Čabala, Head of the Toxicology Department at the General University Hospital in Prague, presents work on the potential utility of GC-TOFMS analysis of cellular fatty acid methyl esters (FAMEs) in identifying clinically relevant bacteria.

Column Choice: A Critical Factor for Successful UHPLC Integration

Column choice is a critical factor in successfully transferring methods between UHPLC and HPLC. Here, we discuss the column qualities that contribute to the successful integration of UHPLC technology.

Determining Pesticides in Dietary Supplements with QuEChERS Extraction, Cartridge SPE, and GCxGC-TOFMS

The novel approach used here combines QuEChERS extraction, cartridge SPE cleanup, and GCxGC-TOFMS analysis, resulting in good recoveries for a wide range of pesticides in dietary supplements. Matrices include dandelion root, sage, and a multi-herb finished product.
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Developing New Methods for Pesticides in Dietary Supplements

QuEChERS is a simple, effective approach to sample prep that can be applied to the analysis of pesticides in dietary supplements. Here, we demonstrate a QuEChERS, cSPE, GC-TOFMS procedure that results in good recoveries for a wide range of pesticides in dandelion root. (PDF - 0kB)
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Dissecting Raptor LC Columns: A closer look at a new species

When we engineered our superficially porous particle (SPP or "core-shell") Raptor LC columns, we developed the bonding chemistries that are best suited to both the SPP construction and our highly selective USLC phases. But we didn't stop here. Take a closer look at a new species as we dissect the upgraded hardware and new, proprietary packing techniques behind Raptor LC columns and Raptor EXP guard columns. (PDF - 0kB)
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Excellent LC-MS Separation of Penicillins and Cephalosporins Using Ultra IBD Columns

Unlike C18 columns, Ultra IBD (intrinsically base deactivated) columns can interact in normal phase mode with analytes that possess charged functional groups, providing greater versatility for LC-MS analyses. Excellent peak shape in either normal phase mode or reversed phase mode increases sensitivity and improves quantification. The 4-page note shows example analyses of penicillins and cephalosporins. (PDF - 0kB)

Fast Screening of Recalled Tylenol for Tribromoanisole and Related Adulterants Using QuEChERS and GC-TOFMS

Screening methods for consumer product adulteration cases, such as the recent Tylenol recall, can benefit from fast QuEChERS-based sample preparation and sensitive, full mass-range GC/TOF-MS.

High-Quality Analysis of Pesticides in Cannabis Using QuEChERS, Cartridge SPE Cleanup, and GCxGC-TOFMS

As medical marijuana is more frequently prescribed, patient safety must be ensured. Pesticide residue testing is an important part of assuring safe product is dispensed, but analysis can be extremely challenging due to matrix complexity. The use of QuEChERS, cartridge SPE cleanup, and GCxGC-TOFMS as presented here produces high-quality quantitative data for this difficult analysis.
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How Column Inertness Improves the Chromatography of Basic Compounds

Not all column deactivations are appropriate for analyzing basic compounds. Here, we demonstrate the effect of column inertness on peak shape and discuss its role in improving method accuracy, sensitivity, and development time. (PDF - 0kB)

How do intrinsically base-deactivated phases work?

Analyzing basic compounds can be somewhat troublesome on traditional alkyl stationary phases, namely conventional C18 columns. This is largely due to the interaction of analyte molecules with silanol groups present on the silica surface. To better understand the workings of silanol interactions, it is important to consider the composition of the support material. Silica is the most commonly used support in the production of HPLC columns, mainly because it is well-suited to high-pressure chromatographic separations, giving high efficiencies and good reproducibility. Silica offers bed and pressure stability and is highly porous, which ultimately gives rise to its large surface area, increased bonding capacity and high peak efficiencies. Silica also possesses widely-studied and effective bonding chemistries, making possible diverse analyte selectivities through a wide variety of bonded stationary phases.

Influencing Selectivity in LC-MS Peptides Analysis on the Raptor ARC-18 Column

Methods for LC-MS peptide analysis often use acidified mobile phases, which can alter retention and selectivity. Here, we demonstrate the effects of modifying acid type, acid concentration, temperature, and gradient slope using several test probes. A Raptor ARC-18 column was employed for this work because it is sterically protected making it extremely stable and resistant to acid damage at low pHs, which is an important characteristic when developing LC-MS methods for peptide analysis.

Novel Column Chemistry—High Impact, Low Cost Technology

Novel column chemistries are a simple change in an already budgeted consumable that can lead to optimized and more reliable methods—giving a fast return on a minimal investment.

Optimized RP-HPLC Method for Hydroxybenzoic Acids

Among hydroxybenzoic acids, hydroxyl groups on the benzene ring vary by position and number, creating differences in overall polarity and solubility. The unique bonding chemistry of the Ultra Aqueous C18 phase assures high resolving power, the best separations across a broad range of analyte polarity, and compatibility with 100% aqueous mobile phases.

Organic Volatile Impurities: Retention Time Index

To make column selection for residual solvents easy, Restek has benchmarked the ICH Class 1, 2 and 3 residual solvents on our most popular OVI columns.
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Colonnes “core-shell” Raptor™ Biphenyl

Les colonnes Raptor™ Restek associent la rapidité des analyses avec le pouvoir de résolution liée à la grande sélectivité des colonnes USLC. La phase Biphenyl est particulièrement appréciée pour son aptitude à séparer les composés pour lesquels les phases C18 ou de type phényl ne sont pas assez résolutives ou rétentives. Les colonnes Raptor™ s’avèrent extrêmement utiles pour obtenir des séparations rapides mettant en œuvre des analyses de substances médicamenteuses ou leurs métabolites. (PDF - 0kB)
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Residual Solvent Analysis: Implementing USP <467>

This 12-page reference includes a of headspace fundamentals, the revised USP <467> method (July, 2008), chromatography for Procedures A, B, and C, and technical tips for optimization. Guidance on fast, effect method development is given. (PDF - 0kB)

Revised USP 467 Residual Solvent Method

The United States Pharmacopeia recently revised the general chapter on residual solvent analysis, USP <467>, to mirror the International Conference on Harmonization (ICH) guidelines for the identification, control and quantification of residual solvents. This revision, effective July 1, 2007, replaces previous methods that were not consistent with the ICH guidelines. Here we provide an overview, chromatograms, and technical tips for successfully running the new procedure.
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Rxi-624Sil MS Columns—Exceptionally Inert, Low Bleed Columns for Volatiles Analysis

Analyze volatile compounds and polar analytes with greater confidence using Rxi-624Sil MS columns. Optimized selectivity, higher inertness, and lower bleed result in reliable separations and accurate, trace-level determinations. Includes environmental and pharmaceutical applications. (PDF - 0kB)

Separating NSAIDs through Aromatic Selectivity

Non-steroidal anti-inflammatory drugs (NSAIDs) are typically separated on C18 phases. Separations on our Allure® Biphenyl HPLC column are based on pi-pi interactions, resulting in optimized retention and selectivity. Increased retention requires higher organic content in the mobile phase, increasing desolvation efficiency in LC/MS. Simple mobile phase changes enhance selectivity, making this column a great alternative to conventional phenyl phase columns, especially in method development.

Two Options for Analyzing Potential Genotoxic Impurities in Active Pharmaceutical Ingredients

Two options for the analysis of PGIs in API have been developed by Merck and Restek to meet different laboratory needs. The first option is a fast method for the analysis of sulfonate esters on the Rxi®-5Sil MS column. The second option is a comprehensive method for the analysis of both sulfonate esters and alkyl halides on the Rtx®-200 column. Both methods require very little sample preparation, which helps increase laboratory productivity.
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USLC Column Selection & Mobile Phase Adjustment Guide

USLC columns and this guide will help you easily choose the right stationary phase to target nearly any analyte in reversed phase or HILIC method development. It will also help you adjust your mobile phase to further improve results without guesswork or wasted time. (PDF - 0kB)

USLC Columns Put the Right Tools in Your LC Method Development Toolbox

Column selectivity has the most significant influence on chromatographic peak separation, or resolution, so choosing the right column can greatly speed up HPLC and UHPLC method development. In this article, we discuss column choice and identify a set of just 4 stationary phases—Restek’s USLC column set—that encompasses the widest range of reversed phase selectivity available today.
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USLC Columns: Choose Columns Fast. Develop Methods Faster.

Restek USLC columns offer the widest range of selectivity available and are an integral part of successful method development. Ideal for column switching systems, these columns provide orthogonal separations to create optimal resolution and robust methods—all in a 4-column set. (PDF - 0kB)