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Analytical methods are developed at various stages of the drug develoment process for samples of varying complexity.

Pharmaceutical 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.

Despite recent advances in column technology and stationary phase chemistry, challenges still remain for routine method development and LC/MS applications.

Method validation is a demanding activity. It requires a large investment in personnel, materials, instruments, supervision, and, most of all, time.

Following its premiere in 2009, it has been announced that the second analytica Vietnam will be held from 7?9 April 2011.

With recent research, the University of Oviedo's analytical spectrometry research group has taken a step closer to the absolute quantification of proteins. Quantification based upon isotope dilution mass spectrometry of sulfur is hampered by gas-based polyatomic interferences. By implementing a quadrupole inductively coupled mass spectrometer with collision/reaction cell technology, the group has been able to overcome the issues and has increased reliability while optimizing the efficiency of its analyses.

An effective metabolite identification study should ideally include both qualitative and quantitative information that for both identifying metabolites, and determining the rate of clearance and the metabolic routes of the parent drug. Liquid chromatography–mass spectrometry (LC–MS) is considered the standard analytical technique for metabolite identification studies. To date, however, qualitative and quantitative information has always been obtained from two separation platforms: quadrupole time-of-flight (QTof) MS for the exact mass full-scan qualitative study, and tandem quadrupole MS for the multiple reaction monitoring (MRM) quantitative study. With advancements to QTof instrumentation, specifically, recent improvements in sensitivity and dynamic range, it is now possible to perform both qualitative and quantitative experiments on a single QTof mass spectrometer. This article describes a workflow that allows simultaneous qualitative and quantitative metabolite identification studies to be..

Flash Directions

A new time-of-flight mass spectrometer was evaluated for performing simultaneous metabolic stability measurement and metabolite identification with ultrahigh-pressure liquid chromatography. Six representative compounds (clomipramine, diclofenac, imipramine, haloperidol, verapamil, and midazolam) were incubated in rat liver microsomes at a more physiologically relevant substrate concentration (1 ?M). High-resolution full-scan and product-ion spectra were acquired in a single injection using generic methodology. Quantitative clearance of the parent was measured using the full-scan data. Major metabolites were identified using the accurate mass product ion spectra. High scanning speed allowed for a sufficient number of data points to be collected across the chromatographic peak for quantitative analysis. Sensitivity was sufficient for obtaining meaningful kinetics with a 1 ?M initial substrate concentration.

This article introduces the advantages of accurate mass high-resolution mass spectrometry LC–MS (HRMS) coupled to the dried blood spot (DBS) technique for fast PK applications in a discovery environment. Compared with the established norm of plasma bioanalysis using triple quadrupoles, HRMS coupled to DBS is a viable alternative. The benefit is access to critical new information (HRMS bioanalysis) and significantly less stress on the animal (DBS), both factors that potentially improve the quality of early PK data.

The threat to human health posed by the recent oil spill has created a pressing need for high-throughput seafood analysis to ensure that it does not contain dangerous levels of polycyclic aromatic hydrocarbons (PAHs) and to allow the earliest possible reopening of the fisheries. Adapting QuEChERS sample preparation technology to this application, combined with the use of preconfigured PAH gas chromatography–mass spectrometry analysis systems, can provide the ability to process in a timely manner the enormous number of samples that will be generated by the ongoing testing program.

The development of a phosphorylation probability scoring tool in an automated data search engine resolves ambiguity in site localization when compared to manual methods.

A high-throughput LC–MS method using core-shell UHPLC columns to screen for a panel of 11 drugs of abuse (expanded SAMHSA) was developed. The corresponding SPE method allowed the reproducible separation and quantitation of these 11 components in less than 2 min. This method demonstrates the power of new-generation HPLC media as well as some of the factors one must consider when developing such methods for LC–MS analysis.

The analysis of urine for drugs of abuse via chromatographic methods is commonplace but can be complicated by high matrix effects and frequent coelution. Novel time-of-flight mass spectrometry in combination with sophisticated deconvolution software was tested and found to provide increased confidence in results due to the high sensitivity and quality of spectra achieved.

The LCGC Awards have now been in existence since 2008, and with several years of award winners now active in the chromatography community, it is fair to say that we now have a reasonable track record and body of work to review in measuring the impact these awards have had, both on the industry and on the winners themselves.

Click the title above to open the LCGC North America October 2010 regular issue, Vol 28 No 10, in an interactive PDF format.

Click the title above to open the October 2010 issue of Current Trends in Mass Spectrometry, Volume 8, Number 4, in an interactive PDF format.

Waters Corporation

New indicators of plant health have been identified by gas chromatography that could provide a remote method for identifying plants that are under attack from pests.

Agilent Technologies has announced that Maquet of Ardon, France, has purchased the company?s OpenLAB ELN electronic lab notebook bundled with Surety's AbsoluteProof third-party, digital timestamping service.

An affiliate of New Mountain Capital announced the completion of its acquisition of Mallinckrodt Baker from Covidien for approximately $280 million.

Thermo Fisher Scientific is sponsoring the 15th Desty Memorial Lecture for Innovation in Separation Science, which will take place at the Royal Institution of Great Britain on the 6th October 2010.

Knauer Application note

Antec application note

Waters Xevo TQ-S is designed for the most demanding quantitative UPLC/MS/MS applications. Using direct injection on Xevo TQ-S removes sample preparation and enables a simple, high-throughput analysis of pesticides in drinking water.

The second Kuwait Laboratory Technology Conference and Exhibition will be held 30 November?1 December 2010.

CTE acquired exclusive manufacturing and marketing rights for novel Cinchona alkaloid-based zwitterion-exchange type chiral stationary phases (CSPs), invented and developed by researchers at the University of Vienna.

Agilent Technologies has announced that a group of researchers from the University of California, Davis, USA, has found that human breast milk contains an unexpected abundance of sugars that coats the lining of infants? intestines, protecting it from noxious bacteria.