Automated sample preparation

The quahty of an analytical result also depends on the vaUdity of the sample utilized and the method chosen for data analysis. There are articles describiag Sampling and automated sample preparation (see Automated instrumentation) as well as articles emphasizing data treatment (see Chemometrics Computer technology), data iaterpretation (see Databases Imaging technology), and the communication of data within the laboratory or process system (see Expert systems Laboratory information managet nt systems). 

I. Fener, V. Pichon, M-C. Hennion and D. Barcelo, Automated sample preparation with exti action columns by means of anti-isoproturon immunosorbents foi the determination of phenylurea herbicides in water followed by liquid chi omatography-diode aixay detection and liquid cliromatogi aphy-atmospheric pressure chemical ionization mass spectrometiy , 7. Chromatogr. 777 91-98 (1997). 

K. Ki onkvist, M. Gustavsson, A.-K. Wendel and H. Jaegfeldt, Automated sample preparation foi the determination of budesonide in plasma samples by liquid chi omatography and tandem mass specti ometi y , 7. Chromatogr. A 823 401-409 (1998). 

Major advantages of LVI methods are higher sensitivity (compare the 100-1000 iL volume in LVI to the maximum injection volume of about 1 iL in conventional splitless or on-column injection), elimination of sample preparation steps (such as solvent evaporation) and use in hyphenated techniques (e.g. SPE-GC, LC-GC, GC-MS), which gives opportunities for greater automation, faster sample throughput, better data quality, improved quantitation, lower cost per analysis and fewer samples re-analysed. At-column is a very good reference technique for rapid LVI. Characteristics of LVI methods are summarised in Tables 4.19 and 4.20. Han-kemeier [100] has discussed automated sample preparation and LVI for GC with spectrometric detection. 

Application Note, The ASPEC System Automated Sample Preparation with Extraction Columns, Gilson Medical Electronics, Middleton, WI (1989). 

ASPEC Automated sample preparation with extraction cartridges... 

Figure 5.1 Flow diagram of the automated sample preparation and instrumental cell isolation equipment.

Deng, Y., Wu, J., Lloyd, T.L., Chi, C.L., Olah, T.V., Unger, S.E. (2002). High-speed gradient parallel liquid chromatography/tandem mass spectrometry with fully automated sample preparation for hioanalysis 30 seconds per sample from plasma. Rapid Commun. Mass Spectrom. 16, 1116-1123. 

Figure 9. Cepheid GeneXpert for automated sample preparation and PCR analysis. (www.Cepheid.com March 18, 2004).

Taylor M.T., Belgrader P., Joshi R., Kintz G.A., Northrup M.A., Fully automated sample preparation for pathogen detection performed in a microfluidic cassette. In Micro Total Analysis Systems 2000, Berg, A. van den, Olthuis, W., Bergveld, P., eds. Kluwer Academic Publishers, The Netherlands, pp 670-672, 2000. 

Kato K. et al., 2005. Determination of 16 phthalate metabolites in urine using automated sample preparation and onhne preconcentration/high-performance liquid chromatography/tandem mass spectrometry. Anal Chem 77 2985. 

Lant M.S. and Oxford J., 1987. Automated sample preparation online with thermospray high-performance liquid chromatography-mass spectrometry for the determination of drugs in plasma. J Chromatogr A 394 223. 

High-Throughput Approaches to Automated Sample Preparation.322... 

Provides a systematic description of high-throughput analysis for the pharmaceutical industry, including advanced instrumentation and automated sample preparation... 

As a consequence of the development of extraction methods for STA based on mixed-mode SPE columns, as well as of the recent introduction of instruments for the automated sample preparation allowing efficient evaporation and derivatization of the extracts, full automation of STA methods based on GC-MS analysis is also available. It needs GC-MS instalments equipped with an HP PrepStation System. The samples directly injected by the PrepStation are analyzed by full scan GC-MS. Using macrocommands, peak identification and reporting of the results are also automated. Each ion of interest is automatically selected, retention time is calculated, and the peak area is determined. All data are checked for interference, peak selection, and baseline determination. 

CF-IRMS provides reliable data on micromoles or even nanomoles of sample without the need for cryogenic concentration because more of the sample enters the ion source than in DI-IRMS. CF-IRMS instruments accept solid, liquid, or gaseous samples such as leaves, soil, algae, or soil gas, and process 100-125 samples per day. Automated sample preparation and analysis takes 3-10 min per sample. The performance of CF-IRMS systems is largely determined by the sample preparation technology. A variety of inlet and preparation systems is available, including GC combustion (GC/C), elemental analyzer, trace gas pre-concentrator and other. The novel... 

For the application of biomolecular NMR in the process of hit identification and hit validation, four important components have to be optimized (i) supply of the target molecule, (ii) selection of ligands, (iii) hardware for automated sample preparation and high-sensitivity measurements, and (iv) software tools for automated data evaluation. 

With the advent of API sources, LC/MS/MS allows the facile development of quantitative methods that are sensitive, selective, robust, and amenable to the rapid analysis of a majority of small molecules. In order to achieve high-throughput bioanalysis in support of pharmacokinetic studies, many approaches have been reported utilizing automated sample preparation and reducing analysis time by pooling samples, parallel analysis, and fast chromatography. 25,26,152,153... 

O Connor, D. Automated sample preparation and LC-MS for high-throughput ADME quantification. Curr Opin Drug Discov Dev 2002, 5, 52-58. 

C. L. Olah, T. V. et al. High-speed gradient parallel liquid chromatography/tandem mass spectrometry with fully automated sample preparation for bioanalysis ... 

Two new ways of automating sample preparation have been commercially exploited firstly the infra-red reflectance techniques, which avoid much of the sample pretreatment required for conventional analysis, and, secondly, robotics, to fully automate or mechanize manual techniques. 

The information in this chapter applies specifically to the first element sample preparation. The sample preparation steps are usually the most tedious and labor-intensive part of an analysis. By automating the sample preparation, a significant improvement in efficiency can be achieved. It is important to make sure that (1) suitable instrument qualification has been concluded successfully before initiation of automated sample preparation validation [2], (2) the operational reliability of the automated workstation is acceptable, (3) the analyte measurement procedure has been optimized (e.g., LC run conditions), and (4) appropriate training in use of the instrument has been provided to the operator(s). The equipment used to perform automated sample preparation can be purchased as off-the-shelf units that are precustomized, or it can be built by the laboratory in conjunction with a vendor (custom-designed system). Off-the-shelf workstations for fully automated dissolution testing, automated assay, and content uniformity testing are available from a variety of suppliers, such as Zymark (www.zymark.com) and Sotax (www.sotax.com). These workstations are very well represented in the pharmaceutical industry and are all based on the same functional requirements and basic principles. 

When creating an automated sample preparation to mimic or reproduce a manual sample preparation procedure, it is wise to break down each step of the procedure and understand its relevance. When transferring the manual steps to automated steps, not every step must or can be transferred individually. For example, when developing a method there might be volume restrictions due... 

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