Biological, Medical, and Clinical Analysis

Novel analytical methods for the discovery and trace analysis of biochemically active compunds in three main area are described: protein analysis, screening technologies and multidimensional separations.

October 2006. The authors demonstrate the use of multiple-injection affinity capillary electrophoresis (MIACE) and several variations to MIACE to determine binding constants between the glycopeptide antibotics vancomycin, ristocetin, and teicoplanin from Streptomyces orientalis, Nocardia lurida, and Actinoplanes teichomyceticus, respectively, and D-Ala-D-Ala terminus peptides.

LabLogic Systems have been chosen by the Department of Medical Physics and Clinical Engineering at Addenbroke's Hospital in Cambridge, UK to supply the equipment to support the department?s metabolite analysis system for early-phase PET studies.

BioTek Instruments has appointed Millennium Science as their official distributor in New Zealand. Millennium Science will now be responsible for sales and support of the company?s entire line of microplate-based instrumentation and software in New Zealand and Australia.

American life sciences company Promega, has opened a new EuroLab facility in Charbonnières near Lyon, France. The laboratory will be used to develop new applications to address Europe?s scientific needs.

The Biotechnology and Biological Sciences Research Council (BBSRC) is launching a consultation on Next Generation Sequencing Technologies. The council is seeking comments from individuals and organizations from the UK?s academic and industrial research community about the potential impacts that these technologies can have on research in biosciences.

A provider of contract laboratory services and manufacturer of scientific instruments in the US, has opened a new European laboratory and office in Warwickshire, UK.

Achieving Product Ion Confirmation

Faculty of Health Sciences at the University of Copenhagen will open the doors of its new research centre, The Novo Nordisk Foundation Centre for Protein Research. The centre is the result of an historic donation from the Novo Nordisk Foundation, which in 2007 gave the university €80 million for its establishment.

PerkinElmer and LEAP Technologies have entered into a resale agreement for ultra high performance liquid chromatography (UHPLC) and high performance liquid chromatography (HPLC) technology.

Presented here are four types of evaporation-free extractions that are widely applicable.

A rapid and simple high performance liquid chromatography (HPLC) method with basic extraction assays was developed to investigate free diazepam levels in the plasma and urine samples of patients medicated with this drug for the management of alcohol withdrawal syndrome. The HPLC analysis was optimized and evaluated for linearity, imprecision, recovery, detection and quantification limits. The method showed linearity between 50–500 ng/mL (r2 ≥ 0.990). Coefficients of variations (%CV) were calculated to be in the range of 1.77–9.60. According to ICH guidelines, theoretical limits of detection (LOD) and quantification (LOQ) for plasma and urine were calculated as 8.3 ng/mL, 27.5 ng/mL and 8.2 ng/mL, 26 ng/mL respectively. Diazepam monitoring in plasma and urine displayed remarkable variations. The importance of adjusting doses according to individual requirements and the routine monitoring of plasma or urine for patients under medication is highlighted.

This column discusses the similarities and differences between the validation approaches for analytical methods for QC product analysis and bioanalysis.

ERLIC is a new technique that shows promise as an alternative or complementary technique for both enrichment and separation of these posttranslationally-modified peptides.

The authors examine MS-based methods to search for protein biomarkers of prion diseases from plasma samples.

Guest authors show how mixed modes can be used successfully in the optimization of protein purification, and discuss how various experimental parameters can be used to regulate the binding of proteins to mixed-mode sorbents.

Microextraction by packed sorbent (MEPS) is a new technique in sample preparation that can be connected on-line to gas chromatography (GC) or liquid chromatography (LC) without any modifications.

A highly sensitive analytical method for the analysis of tamsulosin in human plasma has been developed for use in bioanalytical studies. The solid-phase extraction (SPE) and UPLC–MS–MS methodologies are described, as well as performance against validation parameters.

Technological changes affecting how we access information - both in the depth of knowledge we can access and the speed - leads to some observations about electronic versus print media. First, anything committed to public view must be of high scholarly order, often serving as a prime resource for equations and things we can't or won't remember. Second, once words have been printed, the value of the meaning they impart decreases as new understanding takes shape.

Cytosine (chemical name 4-amino-2-hydroxypyrimidine) is a pyrimidine derivative with a hetereocyclic aromatic ring and two substituents (amine and keto groups) attached and is a polar compound of significant biological and pharmaceutical interest. In response to the intended use of bulk cytosine as a raw material in pharmaceutical manufacturing, a method for the determination of the purity of cytosine was developed.

Part III concludes the print version of our three-part series, "A Mass Spectrometry Primer," with the glossary to follow in a fourth and final installment.

While the "Validation Viewpoint" column has focused on conventional and recombinant pharmaceutical products, and at times, bioanalytical methods, we have just begun to think about method validation as it relates to -omics type studies.

This installment of SPP will compare and contrast the various types of polymeric and non-polymeric sorbents. The major advantages or polymeric sorbents will be discussed, and some applications will illustrate the versatility of polymeric SPE.

The combination of reversed-phase high performance liquid chromatography (RP-HPLC), atmospheric pressure ionization (API), mass spectrometry (MS) and tandem mass spectrometry (MS/MS) is ideal for determining and characterizing analytes in complex biological matrices. This review looks at the importance of parameters such as hydrophobicity, ionization properties, molecular mass and, partially, the molecular structure resulting from applied LC–MS–MS systems in analytical laboratories. The use of these parameters to investigate biomolecules and their unambiguous identification is also described.

The combination of reversed-phase high performance liquid chromatography (RP-HPLC), atmospheric pressure ionization (API), mass spectrometry (MS) and tandem mass spectrometry (MS/MS) is ideal for determining and characterizing analytes in complex biological matrices. This review looks at the importance of parameters such as hydrophobicity, ionization properties, molecular mass and, partially, the molecular structure resulting from applied LC–MS–MS systems in analytical laboratories. The use of these parameters to investigate biomolecules and their unambiguous identification is also described.

Event News

The use of mass spectrometry (MS) in clinical diagnosis goes back to the early 1970s with the application of gas chromatography (GC)–MS to the determination of a variety of biologically significant molecules. Because GC requires a certain level of analyte volatility, and since most biologically active molecules are polar, thermolabile, and involatile, elaborate extraction and derivatization protocols needed to be devised to make GC–MS useful for the analysis of clinically relevant samples. To make sample analysis less difficult by MS there had been a significant amount of R&D invested over several decades aimed at coupling high performance liquid chromatography (HPLC) with MS since HPLC is a much better separation technology than GC for polar thermolabile biologically relevant molecules. This coupling was not without significant challenges; most of the LC–MS coupling techniques that evolved during the 1970s and 1980s were not very successful, and many of those that enjoyed some widespread..

Microemulsion liquid chromatography (MELC) is a recent development offering reduced sample preparation times for complex samples and generic separation conditions applicable to a wide range of solutes. This article introduces the concepts of MELC and discusses the possible benefits and future applications.

The 25th anniversary of the Montreux LC–MS symposium will be held at the Montreux Music and Convention Centre, Montreux, Switzerland from 12–14 November 2008.

Micellar liquid chromatography (MLC) is a reversed-phase liquid chromatographic mode with a solution of surfactant forming micelles as the mobile phase. The interaction of solutes with the stationary phase coated with surfactant monomers, combined with the increased solubilization capability of micelles, have profound implications with regard to retention, selectivity and efficiency. Practical steps that a chromatographer involved in MLC should consider when developing an analytical procedure are described, including mobile phase preparation, column conditioning and cleaning.