Skip to main content Accessibility help
×
Hostname: page-component-78c5997874-ndw9j Total loading time: 0 Render date: 2024-11-06T02:03:09.428Z Has data issue: false hasContentIssue false

5 - The importance of a quality assurance plan for method validation and minimizing uncertainties in the HPLC analysis of phytoplankton pigments

Published online by Cambridge University Press:  05 March 2012

Suzanne Roy
Affiliation:
Université du Québec à Rimouski, Canada
Carole A. Llewellyn
Affiliation:
Plymouth Marine Laboratory
Einar Skarstad Egeland
Affiliation:
University of Nordland, Norway
Geir Johnsen
Affiliation:
Norwegian University of Science and Technology, Trondheim
Get access

Summary

Introduction

A quality assurance plan (QAP) describes a process to ensure an analytical method fulfils the agreed upon accuracy objectives at all points during the analysis of samples. A QAP includes such things as standardized procedures, method validation, quality control (QC) measurements, and quality assessment (QA); the latter quantitatively describes how results of QC measurements are used to determine whether a method is performing within expectations. By analogy, a QAP describes what can be considered, in a more general sense, a ‘holistic’ approach to sample analysis, whereby the ‘whole is considered to be a result of the interdependence of all parts’. Here, the ‘whole’ represents the overall combined uncertainty of a final data product, and ‘the interdependence of all parts’ represents the uncertainties contributed by the many individual procedures required to produce that final data product.

An in depth discussion of uncertainty analysis in the chemical laboratory, given in EURACHEM (2000), is beyond the scope of this chapter, but the importance of a so-called holistic approach to sample analysis, whether this includes a formalized QAP or not, is necessary to provide knowledge of the uncertainties associated with measured values and, thus, facilitate confidence in the data products. Such knowledge is important, because pigment data are often compiled in increasingly large databases, and end users of the data are remote (in space and time) from the data providers. Knowing the accuracy of the data facilitates their wider utility, for both current and unanticipated future applications. This chapter describes components of a QAP in the context of knowledge gained during intercomparisons sponsored by the National Aeronautics and Space Administration (NASA). A primary objective of these activities was to determine if the myriad providers of HPLC analyses to NASA researchers were satisfying the accuracy requirements for field observations.

Type
Chapter
Information
Phytoplankton Pigments
Characterization, Chemotaxonomy and Applications in Oceanography
, pp. 195 - 256
Publisher: Cambridge University Press
Print publication year: 2011

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Barlow, R. G.Mantoura, R. F. C.Gough, M. A.Fileman, T. W. 1993 Pigment signatures of the phytoplankton composition in the northeastern Atlantic during the 1990 spring bloomDeep-Sea Res. II 40 459CrossRefGoogle Scholar
Bidigare, R. R.Ondrusek, M. E. 1996 Spatial and temporal variability of phytoplankton pigment distributions in the central equatorial Pacific OceanDeep-Sea Res. II 43 809CrossRefGoogle Scholar
Bidigare, R. R.Van Heukelem, L.Trees, C. C. 2003 HPLC phytoplankton pigments: sampling, laboratory methods and quality assurance proceduresOcean Optics Protocols for Satellite Ocean Color Sensor Validation, Revision 4, Volume V: Biogeochemical and Bio-optical Measurements and Data Analysis ProtocolsMueller, J. L.Fargion, G. S.McClain, C. L.GreenbeltNASA Goddard Space Flight Center5Google Scholar
Bidigare, R. R.Van Heukelem, L.Trees, C. C. 2005 Analysis of algal pigments by high-performance liquid chromatographyAlgal Culturing TechniquesAndersen, R.BurlingtonElsevier Academic Press327Google Scholar
Castells, C. B.Castells, R. C. 1998 Peak distortion in reversed-phase liquid chromatography as a consequence of viscosity difference between sample solvent and mobile phaseJ. Chromatogr. A 805 55CrossRefGoogle Scholar
Claustre, H. 1994 The trophic status of various oceanic provinces as revealed by phytoplankton pigment signaturesLimnol. Oceanogr 39 1206CrossRefGoogle Scholar
Claustre, H.Hooker, S.B.Van Heukelem, L.Berthon, J. F.Barlow, R.Ras, J.Sessions, H.Targa, C.Thomas, C. S.van der Linde, D.Marty, J-C. 2004 An intercomparison of HPLC phytoplankton pigment methods using samples: application to remote sensing and database activitiesMar. Chem 85 41CrossRefGoogle Scholar
Clesceri, L. S.Greenberg, A. E.Eaton, A. D. 1998 Part 1020, Quality Assurance, Section 1020C, Quality Assessment in Standard Methods for the Examination of Water and WastewaterBaltimoreAmerican Public Health Association, American Water Works Association, Water Environment Federation, Baltimore, Maryland1
Dolan, J. W. 1999 Readers’ questions, carryover, mobile-phase temperature, and column careLC GC 20 1006Google Scholar
Dolan, J. W. 2001 Autosampler carryoverLC GC 19 164Google Scholar
Dolan, J. W. 2001 Attacking carryover problemsLC GC 19 1050Google Scholar
Dolan, J. W. 2002 Resolving minor peaksLC GC 20 594Google Scholar
Dolan, J. W. 2006 Autosampler carryoverLC GC 24 754Google Scholar
EURACHEM Guide 1998 The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related TopicsMr. David Holcombe, Drafting Secretary for EURACHEM working Group, LGC, Queens Rd. TeddingtonMiddlesex, TW11 0lYhttp://www.eurachem.org/Google Scholar
EURACHEM/CITAC Guide 2000 Quantifying Uncertainty in Analytical MeasurementEllison, S. L. R.LGC, UKM. Rosslein (EMPA, Switzerland), A. Williams (UK)http://www.eurachem.org/
Gieskes, W. W. C.Kraay, G. W.Nontji, A.Setipermana, D.Sutomo, D. 1988 Monsoonal alternation of a mixed and a layered structure in the phytoplankton of the euphotic zone of the Banda Sea (Indonesia): A mathematical analysis of algal pigment fingerprintsNeth. J. Sea Res 22 123CrossRefGoogle Scholar
Hastie, T.Tibshirani, R.Friedman, J. 2001 The Elements of Statistical Learning: Data Mining, Inference, and PredictionNew YorkSpringer Science+Business Media.CrossRefGoogle Scholar
Helsinki Commission 2006 http://www.helcom.fi/groups/monas/CombineManual/PartB/en_GB/main/
Hooker, S. B.Esaias, W. E. 1993 An overview of the SeaWiFS projectEos, Trans. AGU 74 241CrossRefGoogle Scholar
Hooker, S. B.McClain, C. R. 2000 The calibration and validation of SeaWiFS dataProg. Oceanogr 45 427CrossRefGoogle Scholar
Hooker, S. B.Claustre, H.Ras, J.Van Heukelem, L.Berthon, J. -F.Targa, C.van der Linde, D.Barlow, R.Sessions, H. 2000 The First SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-1)Hooker, S. B.Firestone, E. R.GreenbeltNASA Goddard Space Flight Center.Google Scholar
Hooker, S. B.Van Heukelem, L.Thomas, C. S.Claustre, H.Ras, J.Barlow, R.Sessions, H.Schlüter, L.Perl, J.Trees, C.Stuart, V.Head, E.Clementson, L.Fishwick, J.Llewellyn, C.Aiken, J. 2005 The Second SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-2)GreenbeltNASA Goddard Space Flight Center.Google Scholar
Hooker, S. B.Van Heukelem, L.Thomas, C. S.Claustre, H.Ras, J.Schlüter, L.Clementson, L.van der Linde, D.Eker-Develi, E.Berthon, J. -F.Barlow, R.Sessions, H.Ismail, H.Perl, J. 2009 The Third SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-3)NASA Goddard Space Flight CenterGoogle Scholar
Hooker, S. B.Van Heukelem, L.Thomas, C. S.Schlüter, L.Russ, M. E.Ras, J.Claustre, H.Clementson, L.Canuti, E.Berthon, J -F.Perl, J.Normandeau, C.Cullen, J.Kienast, M.Pinckney, J. L.Millie, D. 2010 The Fourth SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-4)NASA Goddard Space Flight CenterGoogle Scholar
Humphrey, G. G.Jeffrey, S. W. 1997 Appendix G, Tests of accuracy of spectrophotometric equations for the simultaneous determination of chlorophylls , , 1 and 2Phytoplankton Pigments in Oceanography: Guidelines to Modern MethodsJeffrey, S. W.Mantoura, R. F. C.Wright, S. W.ParisUNESCO Publishing616Google Scholar
International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use 2005
International Union of Pure and Applied Chemistry (IUPAC) 1998 Chapter 18, Quality Assurance of Analytical Processes, Section 18.4.3.7Compendium of Analytical Nomenclature: Definitive Rules 1997OxfordBlackwell Sciencehttp://old.iupac.org/publications/analytical_compendium/Google Scholar
Jeffrey, S. W.Humphrey, G. F. 1975 New spectrophotometric equations for determining chlorophylls , , 1 and 2 in higher plants, algae and natural phytoplanktonBiochem. Physiol. Pflanzen 167 191CrossRefGoogle Scholar
Jeffrey, S. W.Wright, S. W. 1997 Qualitative and quantitative HPLC analysis of SCOR reference algal culturesPhytoplankton Pigments in Oceanography: Guidelines to Modern MethodsJeffrey, S. W.Mantoura, R. F. C.Wright, S. W.ParisUNESCO Publishing343Google Scholar
Jeffrey, S. W.Mantoura, R. F. C.Wright, S. W. 1997 Phytoplankton Pigments in Oceanography: Guidelines to Modern MethodsParisUNESCO Publishing
JGOFS 1994 Protocols for the Joint Global Ocean Flux Study Core Measurements 29 Paris, FranceUNESCO Publishing91Google Scholar
King, P. G. 1999 HPLC method development and validation: A direct procedure for determining the linear-through-zero rangeLC GC 6 46Google Scholar
Latasa, M.Bidigare, R. R.Ondrusek, M. E.Kennicutt II, M. C. 1996 HPLC analysis of algal pigments: a comparison exercise among laboratories and recommendations for improved analytical performanceMar. Chem 51 315CrossRefGoogle Scholar
Latasa, M.van Lenning, K.Garrido, J. L.Scharek, R.Estrada, M.Rodríguez, F.Zapata, M. 2001 Losses of chlorophylls and carotenoids in aqueous acetone and methanol extracts prepared for RPHPLC analysis of pigmentsChromatographia 53 385CrossRefGoogle Scholar
Mantoura, R. F. C.Repeta, D. J. 1997 Calibration methods for HPLCPhytoplankton Pigments in Oceanography: Guidelines to Modern MethodsJeffrey, S. W.Mantoura, R. F. C.Wright, S. W.ParisUNESCO Publishing343Google Scholar
Miller, J. N.Miller, J. C. 2000 Statistics and Chemometrics for Analytical ChemistryPearson Education Limited, Prentice Hall PublisherGoogle Scholar
Mueller, J. L. 2000 Overview of measurement and data analysis protocolsOcean Optics Protocols for Satellite Ocean Color Sensor Validation, Revision 2Fargion, G. S.Mueller, J. L.Greenbelt, MarylandNASA Goddard Space Flight Center87Google Scholar
Mueller, J. L. 2002 Overview of measurement and data analysis protocolsOcean Optics Protocols for Satellite Ocean Color Sensor Validation, Revision 3Mueller, J. L.Fargion, G. S.GreenbeltNASA Goddard Space Flight Center123Google Scholar
Mueller, J. L. 2003 Overview of measurement and data analysis methodsOcean Optics Protocols for Satellite Ocean Color Sensor Validation, Revision 4, Volume III: Radiometric Measurements and Data Analysis ProtocolsMueller, J. L.GreenbeltNASA Goddard Space Flight Center1Google Scholar
Mueller, J. L.Austin, R. W. 1992 Ocean Optics Protocols for SeaWiFS ValidationHooker, S. B.Firestone, E. R.GreenbeltNASA Goddard Space Flight CenterGoogle Scholar
Mueller, J. L.Austin, R. W. 1995 Ocean Optics Protocols for SeaWiFS Validation, Revision 1Hooker, S. B.Firestone, E. R.Acker, J. G.GreenbeltNASA Goddard Space Flight CenterGoogle Scholar
Riddick, J. A.Bunger, W. B.Sakano, T. K. 1986 Organic Solvents: Physical Properties and Methods of PurificationNew YorkJohn Wiley & SonsGoogle Scholar
Snyder, L. R.Kirkland, J. J. 1979 Introduction to Modern Liquid ChromatographyNew YorkWileyGoogle Scholar
Taylor, J. K. 1987 Quality Assurance of Chemical MeasurementsChelseaLewis PublishersGoogle Scholar
Trees, C. C.Clark, D. K.Bidigare, R. R.Ondrusek, M. E.Mueller, J. L. 2000 Accessory pigments versus chlorophyll concentrations within the euphotic zone: a ubiquitous relationshipLimnol. Oceanogr 45 1130CrossRefGoogle Scholar
U.S. Department of Health and Human Services, Food and Drug Administration (USDHHS), Center for Drug Evaluation and Research (CDER), ChemistryReviewer Guidance: Validation of Chromatographic Methods 1994 http://www.fda.gov/cder/guidance/cmc3_rev.pdf
U.S. Department of Health and Human Services, Food and Drug Administration (USDHHS), Center for Drug Evaluation and Research (CDER), ICH-Quality 1995 http://www.fda.gov/cder/guidance/ichq2a.pdf
U.S. Department of Health and Human Services, Food and Drug Administration (USDHHS), Center for Drug Evaluation and Research (CDER), Center for Biologics Evaluation and Research (CBER) 1996 http://www.fda.gov/cder/guidance/1320fnl.pdf
U.S. Department of Health and Human Services, Food and Drug Administration (USDHHS), Center for Drug Evaluation and Research (CDER), Center for Veterinary Medicine (CVM) 2001 http://www.fda.gov/cder/guidance/4252fnl.pdf
Van Heukelem, L.Thomas, C. S. 2001 Computer-assisted high-performance liquid chromatography method development with applications to the isolation and analysis of phytoplankton pigmentsJ. Chromatogr. A 910 31CrossRefGoogle ScholarPubMed
Van Heukelem, L.Thomas, C. S.Glibert, P. 2002 Sources of variability in chlorophyll analysis by fluorometry and high-performance liquid chromatography in a SIMBIOS inter-calibration exerciseGreenbeltNASA Goddard Space Flight CenterGoogle Scholar
Zapata, M.Garrido, J. L. 1991 Influence of injection conditions in reversed-phase high performance liquid chromatography of chlorophyll and carotenoidsChromatographia 31 589CrossRefGoogle Scholar

Save book to Kindle

To save this book to your Kindle, first ensure [email protected] is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about saving to your Kindle.

Note you can select to save to either the @free.kindle.com or @kindle.com variations. ‘@free.kindle.com’ emails are free but can only be saved to your device when it is connected to wi-fi. ‘@kindle.com’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

Available formats
×

Save book to Dropbox

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Dropbox.

Available formats
×

Save book to Google Drive

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Google Drive.

Available formats
×