PharmTech LCGC Sciex Webinar 11.10

All News

Pittcon Interviews

John Di Mare, Agilent Account Manager, talks with us about what the company is up to at this year's Pittcon, as well as the acquisition of Varian.

E-Separation Solutions

In this application note, two column pairs were exhibited for organochlorine pesticide analysis. The Zebron ZB-XLB and ZB-35 are traditionally used for this analysis but the Zebron ZB-MultiResidue-1 and -2 pair show additional benefits of improved resolution.

LCGC Europe eNews

Merck and Millipore have announced that the two companies have reached an agreement that will see Merck acquire Millipore for around $7.2 billion.

Acetaminophen (paracetamol; APAP; IUPAC: N-(4-hydroxyphenyl)acetamide) was chosen as model drug to investigate oxidative metabolism using the ROXY EC System dedicated for single component screening. Electrochemical conversion of the acetaminophen into reactive phase I metabolites and the NAPQI ? GSH phase II conjugate was successfully achieved.

The Column

CHROMacademy offers continuing professional development. Tony Taylor spoke to The Column about the benefits this approach offers chromatographers.

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Xevo Family

Waters designed every component of the Xevo? Family with Engineered Simplicity? in mind.

Pittcon 2010 Day 3

All of the most important sessions, awards and events from Pittcon 2010 covered here in this convenient and easy-to-read daily e-newsletter.

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The Application Notebook

There is considerable attention placed on the synthesis and characterization of polypeptoids, a new class of synthetic polypeptide analogues. Because of intense hydrogen-bonding among chains of these polymers, aggressive solvents such as hexafluoroisopropanol (HFIP) must be used as the mobile phase to support solubility.

The Application Notebook

Recent technological advances in macromolecular crystallography led to focus on the study of more and more sophisticated biological systems, such as protein–protein complexes. Nevertheless, they represent one of the most challenging areas in modern structural biology.

The Application Notebook

The procedure involves a rapid and efficient pretreatment with SampliQ QuEChERS kits. The homogenized liver sample was initially extracted in a buffered aqueous/1% acetic acid acetonitrile system with an extraction and partitioning step after the addition of salts. Finally, the sample was cleaned up using dispersive solid-phase extraction (dispersive-SPE). The final extracts were analysed by the sensitive and selective determination of all compounds in a single run using LC–ESI-MS–MS operating in positive ion multiple reaction monitoring (MRM) mode. Sulphapyridine was selected as the internal standard. The accuracy of the method, expressed as recovery, was between 53 and 93%. The precision, expressed as RSD, was between 2.1 and 16.8%. The established 5 ng/g limits of quantification (LOQ) were much lower than the respective maximum residue limit (MRL) for sulphonamide in animal food products (20–100 ng/g).

The Application Notebook

The procedure involves a rapid and efficient pretreatment by SampliQ QuEChERS kits. The homogenized liver sample was initially extracted in a buffered aqueous, 5% formic acid acetonitrile system. An extraction and partitioning step was performed after the addition of salts. Clean-up was done using dispersive solid-phase extraction (dispersive-SPE). The final extracts allowed determination of all compounds in a single run using LC–ESI-MS–MS operating in positive ion multiple reaction monitoring (MRM) mode. Norfloxacin was selected as the internal standard. The accuracy of the method, expressed as recovery, was between 62 and 113%. The precision, expressed as RSD, was between 2.2 and 13.4%. The established limit of quantification (LOQ) was 5 ng/g and is significantly lower than the respective maximum residue limit (MRL) for quinolones in food producing animals.

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The Application Notebook

In the past decade, supercritical fluid chromatography (SFC) has experienced a steady growth in acceptance, particularly in pharmaceutical and chemical laboratories. In SFC, "supercritical" CO2 combined with one or more polar organic solvents, most commonly alcohols, are used as mobile phase. Preparative SFC is deemed by many to hold the greatest promise to attain mainstream acceptance. The reduction in solvent consumption and collection in relatively small volumes of volatile organic solvents, hence, a much less stringent post-purification endeavour, lead to significant savings on operation costs. For example, Ripka et al. calculated that 20000 samples purified by SFC instead of reverse phase liquid chromatography (RPLC) would realize a 48 times reduction in solvent consumption.1

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The Application Notebook

The determination of BTEX in gasoline is usually performed in accordance with the standard test method ASTM D3606 using gas chromatography. However, particularly in the presence of ethanol, co-elutions are observed in one-dimensional chromatography. In this application note a method is described applying multidimensional GC to overcome the separation problem.

The Application Notebook

Viruses are packets of infectious nucleic acid (either DNA or RNA) surrounded by a protective coat consisting of a large number of protein subunits. Because viruses can cause various diseases - some life-threatening - characterizing virus particles thoroughly in terms of their size distribution, aggregation and absolute counts-per-unit volume is of extreme importance.

The Application Notebook

The Agilent 1290 Infinity LC has significant capabilities for a wide range of HPLC and UHPLC applications. It exhibits a broader power range (that is, the combination of pressure and flow capabilities) than any other commercially available system and has the flexibility to operate with a wide range of column dimensions and particle sizes. Additionally, advanced optical design in the diode array detector allows a wide dynamic range and high sensitivity, both of which are critical in the monitoring of small impurities in fine chemicals.

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The Application Notebook

The characterization of pharmaceutical salts is critical to the drug development process. Active pharmaceutical ingredient (API) salts influence the solubility, stability and hygroscopicity of pharmaceuticals and affect the final drug formulation. Traditionally, the analysis of the API and its counterion salt requires separate applications. Nanopolymer silica hybrid (NSH) technology in the Acclaim Trinity P1 column along with the Corona ultra charged aerosol detector (CAD) enables simultaneous analysis of the API and counterion over four orders of magnitude.

Pittcon 2010 Day 2

All of the most important sessions, awards and events from Pittcon 2010 covered here in this convenient and easy-to-read daily e-newsletter.

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The Application Notebook

The stevia plant and its extracts have long been used as sweeteners in Asia and Latin America. Two steviol glycosides present in plant tissue, stevioside and rebaudioside A, are largely responsible for the sweet flavour.1 In December 2008, the US FDA placed rebaudioside A (also known as rebiana) on the Generally Recognized as Safe (GRAS) list of sugar substitutes to be used in foods, thereby allowing the use of rebiana as a commercial sweetener.2 The determination of steviol glycosides in these sweeteners is challenging due to their weak UV absorbance. Other detection methods, such as evaporative light scattering (ELS), can improve steviol glycoside quantification. In this proposed method, steviol glycosides were determined by UV and ELS detections in consumer sweeteners following separation on the Acclaim Mixed-Mode WAX-1 column.3

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The Application Notebook

Polyols are alcohols with multiple hydroxyl groups. They are used for very different applications, such as, for example, in Feed and Food as sugar substitutes or in polymer chemistry as reactants to produce high quality products.

E-Separation Solutions

Wednesday morning?s session, ?Achievements and Challenges in Mass Spectrometry,? was arranged by Imma Ferrer and Michael Thurman of the University of Colorado. Starting out the session will be Thurman with his opening remarks on the state of mass spectrometry.

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The Application Notebook

The combination of the small particle size and narrow particle size distribution coupled with the significantly shorter diffusion path provided by the Kinetex core-shell particle results in a material that yields significantly increased column efficiencies and chromatographic resolution. This is a significant benefit for separation scientists looking to increase efficiency and chromatographic resolution, especially for complex separations containing many compounds and very closely eluting compounds so that accurate identification and quantification can be achieved.

E-Separation Solutions

Good morning, and welcome to the final day of LCGC?s coverage from Pittcon 2010. To say the week has flown by would be an understatement, as I?m sure many conference-goers share our feeling that the conference has been a blur of activity to this point.

E-Separation Solutions

The 2010 Ralph N. Adams Award in Bioanalytical Chemistry will be presented to Catherine Fenselau, Professor of Chemistry and Biochemistry at the University of Maryland (College Park, Maryland), on Wednesday afternoon at Pittcon 2010.

E-Separation Solutions

Wednesday?s Pittcon Audio & Video Theater will be dedicated to CHROMacademy. CHROMacademy is a cutting-edge e-learning programme that LCGC is launching in collaboration with Crawford Scientific. The site will provide continual professional development for chromatographers to make them more effective in the workplace.