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App Notes Pharma
  • Automating Method Development with an HPLC System Optimized for Scouting of Columns, Eluents and Other Method Parameters


    HPLC method development is still considered one of the critical bottlenecks that impedes productivity in analytical laboratories. Because of the variety of available columns and mobile phases applicable in reversed-phase chromatography, the selection of optimal conditions is a challenge. Here we present an integrated LC system and software that automatically screens possible combinations of columns, mobile phases and temperatures.

    GPC/SEC Analysis of Mono-, Di-, Triacylglyceride and Glycerol According to European Pharmacopoeia


    Mono-, di-, triacylglyceride are widely used as emulsifiers in food and pharmaceutical industries. Some paints and adhesives may also contain different glyceride samples.

    On-Line Sample Clean-Up for the LC–MS Analysis of Small Molecules in Serum


    Drug discovery/detection commonly focuses on analytes which are present in biological matrices. Direct injection of such samples onto LC and LC–MS systems is problematic as analytes of interest can be "lost" in the concentrated matrix peak, plus instrument and column contamination readily occurs.

    Determination of Paromomycin in a Bulk Pharmaceutical Formulation Using HPAE-IPAD


    Comparing Manual Compound Optimizations Against Automated Optimizations Obtained by QuickQuan on the TSQ Quantum Access


    One of the rate limiting steps in LC–MS–MS sample analysis is the time required to create accurate and sensitive instrument methods. To ensure the best possible performance, operators may spend an extended period of time optimizing the mass spectrometer for compounds of interest. In laboratories where higher throughput is required, the allotted time for instrument optimization is minimal. Automated optimization packages are frequently used to increase throughput, but these solutions compromise assay sensitivity for the sake of speed.

    Developing a Fast, Generic Method for Rapid Resolution LC with Quadrupole MS Detection


    The Agilent 6140 quadrupole LC–MS, equipped with the multimode source and combined with an Agilent 1200 Series Rapid Resolution LC system was used to develop a fast, generic LC–MS method for the analysis of 35 pharmaceutical compounds from 17 compound classes. Through further optimization the method run time was reduced from 2.1 to 0.8 minutes without compromising chromatographic quality.

    Pushing the Boundaries: Employing Phenomenex's HILIC, RP and Traditional Normal-Phase Columns for SFC Analysis and Purification


    Analyses and purifications of reaction mixtures are among the most demanding tasks for analytical chemists in the pharmaceutical industry. This is especially true during the hit-to-lead and lead optimization stages of drug discovery. Today's complicated synthetic routes can generate complex mixtures with a wide range of polarities and functionalities. Currently, the predominant chromatographic tool for resolving these mixtures is liquid chromatography (LC), particularly reverse phase LC (RPLC).

    Extraction of Polar Basic Drugs from Plasma with Polymeric SPE Cation Exchange, Bond Elut Plexa PCX


    Basic pharmaceutical drugs are ideal for extraction with a cation exchange sorbent. Analytes are easily charged in an acidic solution and readily interact with the ion exchange functionalities of the sorbent. Polar basic compounds can be problematic for reverse phase sorbents, because of their poor hydrophobic interaction and water solubility.

    Use of an Efficient LC Method Development Approach in the Analysis of Terfenadine, Fexofenadine and Azaclonol


    Using ACQUITY UPLC technology with triple quadrupole MS detection enhances the selectivity, sensitivity and throughput in quantitative bioanalytical studies. Detection limits for these methods are being driven lower and lower as drugs become more potent. For this reason, methods with highest sensitivity possible must be developed. Additionally, this must happen under increasingly tight deadlines to shorten the drug development cycle. We have developed a straightforward, streamlined approach to efficient LC method development. This use of this approach is demonstrated in the generation of a sensitive and selective method for terfenadine and two of its metabolites, fexofenadine and azacyclonol. Fexofenadine, in particular, has gained importance as the commonly prescribed anti-allergic Allegra.

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