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

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) 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 (RSDINST≤1.5%); (2) linearity (R2≥0.998; RSDSENSITIVITY≤4%; REMAX≤8%; REAVER≤ 3%); (3) precision (RSD≤1.5%); (4) trueness (recovery of 97-103%); (5) LOD (≤3mg/L); and (6) LOQ (10mg/L

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

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) 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 (RSDINST 641.5%); (2) linearity (R2 650.998; RSDSENSITIVITY 644%; REMAX 648%; REAVER 64 3%); (3) precision (RSD 641.5%); (4) trueness (recovery of 97-103%); (5) LOD ( 643mg/L); and (6) LOQ (10mg/L)

First international comparative study of volatile fatty acids in aqueous samples by chromatographic techniques: Evaluating sources of error

This first international proficiency-testing scheme evaluated the analytical performance and the state of practice in measurement of volatile fatty acids in aqueous samples. Gas chromatography and high-performance liquid chromatography were used by 25 laboratories from 15 different countries. Two reference materials were selected for analysis. The performance of each laboratory was assessed by the internationally-accepted z-score. The overall performance was rather poor. Among the causes of poor analytical performance, human errors and inadequate calibration were probably the major problems encountered. © 2013 Elsevier Ltd