Harmonization of the quantitative determination of volatile fatty acids profile in aqueous matrix samples by direct injection using gas chromatography and high-performance liquid chromatography techniques: Multi-laboratory validation study

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DOIResolve DOI: http://doi.org/10.1016/j.chroma.2015.08.008
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TypeArticle
Journal titleJournal of Chromatography A
ISSN0021-9673
Volume1413
Article number356775
Pages94106; # of pages: 13
SubjectChromatography; Direct injection; Fatty acids; Parameter estimation; Aqueous matrices; Chromatographic techniques; Interlaboratory studies; Performance parameters; Quantification methods; Quantitative determinations; Volatile fatty acids (VFAs); Volatile fatty acids; volatile fatty acid; aqueous solution; concentration (parameters); controlled study; fatty acid analysis; gas chromatography; high performance liquid chromatography; limit of detection; limit of quantitation; priority journal; quantitative analysis; validation study
AbstractThe performance parameters of volatile fatty acids (VFAs) measurements were assessed for the first time by a multi-laboratory validation study among 13 laboratories. Two chromatographic techniques (GC and HPLC) and two quantification methods such as external and internal standard (ESTD/ISTD) were combined in three different methodologies GC/ESTD, HPLC/ESTD and GC/ISTD. Linearity evaluation of the calibration functions in a wide concentration range (10-1000mg/L) was carried out using different statistical parameters for the goodness of fit. Both chromatographic techniques were considered similarly accurate. The use of GC/ISTD, despite showing similar analytical performance to the other methodologies, can be considered useful for the harmonization of VFAs analytical methodology taking into account the normalization of slope values used for the calculation of VFAs concentrations. Acceptance criteria for VFAs performance parameters of the multi-laboratory validation study should be established as follows: (1) instrument precision (RSD<inf>INST</inf>≤1.5%); (2) linearity (R2≥0.998; RSD<inf>SENSITIVITY</inf>≤4%; RE<inf>MAX</inf>≤8%; RE<inf>AVER</inf>≤ 3%); (3) precision (RSD≤1.5%); (4) trueness (recovery of 97-103%); (5) LOD (≤3mg/L); and (6) LOQ (10mg/L).
Publication date
PublisherElsevier
LanguageEnglish
AffiliationNational Research Council Canada (NRC-CNRC); Energy, Mining and Environment
Peer reviewedYes
NPARC number21276934
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Record identifier9cffbe6a-8f13-413f-af23-a926d21f06bb
Record created2015-11-10
Record modified2016-05-09
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