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.

作者: Francisco Raposo , Rafael Borja , Jesús A. Cacho , Jan Mumme , Ángel F. Mohedano

DOI: 10.1016/J.CHROMA.2015.08.008

关键词: Volatile fatty acidsCalibrationAqueous solutionChemistryGas chromatographyMatrix (chemical analysis)Validation studyChromatographyHigh-performance liquid chromatographyAnalytical chemistryDetection limit

摘要: The 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) two quantification methods such as external internal standard (ESTD/ISTD) combined in three different methodologies GC/ESTD, HPLC/ESTD GC/ISTD. Linearity evaluation calibration functions wide concentration range (10-1000mg/L) was carried out using statistical goodness fit. Both considered similarly accurate. use GC/ISTD, despite showing similar analytical to other methodologies, can be useful harmonization VFAs methodology taking into account normalization slope values used calculation concentrations. Acceptance criteria should established follows: (1) instrument precision (RSDINST≤1.5%); (2) linearity (R(2)≥0.998; RSDSENSITIVITY≤4%; REMAX≤8%; REAVER≤ 3%); (3) (RSD≤1.5%); (4) trueness (recovery 97-103%); (5) LOD (≤3mg/L); (6) LOQ (10mg/L).

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