2019 Volume 67 Issue 1 Pages 59-63
The present study proposes a method for the assessment of repeatability in supercritical fluid chromatography with electrochemical detection (SFC-ECD), based on the ISO 11843 part 7 (ISO 11843-7:2018) which can theoretically provide detection limits and standard deviation (S.D.) through the stochastic properties of baseline noise without repetitive measurements of real samples. On the baseline noise of SFC-ECD, large-amplitude and periodic noises with less than 0.05 Hz were observed, and the power spectrum of the baseline noise showed 1/f fluctuation (f = frequency). It was found that the present power spectrum analysis, according to the law of error propagation, can provide suitable noise parameters to calculate S.D. of baseline noise and a relative S.D. (RSD) of peak area by ISO 11843-7. The chromatographic determinations of α-, β-, γ- and δ-tocopherol have been taken as examples. In the present SFC-ECD, the RSDs of peak areas for α-, β-, γ- and δ-tocopherol obtained by ISO 11843-7 were within 95% confidence intervals of the RSD of them obtained by repetitive measurements (n = 6). Thus, we found that ISO 11843-7 is applicable to the assessment of repeatability in SFC-ECD for determining tocopherols without repetitive measurements.
