Objective: To establish a GC method for simultaneous determination of acetaldehyde, butyraldehyde, crotonaldehyde, tert-butanol, 2-ethylbutyl alcohol, 2-ethylbutyric acid and paraldehyde in 2-ethylbutanal. Methods: GC method was adopted. The determination was performed on capillary column of Aglient DB-1 (30 m×0.53 mm, 3 μm); the column temperature was programmed to start at 60 ℃, maintained for 2 min, and then rose to 120 ℃ at a rate of 5 ℃·min-1, maintained for 15.5 min; inlet temperature was 200 ℃; the temperature of the flame ionization detector was 260 ℃; nitrogen was used as the carrying gas, the split ratio was 40∶1; the injection volume was 1 μL, and quantified by external standard method. Results: The acetaldehyde, butyraldehyde, crotonaldehyde, tert-butanol, 2-ethylbutyl alcohol, 2-ethylbutyric acid and paraldehyde showed good linearity in the ranges of 0.100 1-0.300 4 mg·mL-1(r=0.999 1), 0.200 5-0.601 5 mg·mL-1(r=0.999 4), 0.025 5-0.076 6 mg·mL-1(r=0.999 3), 0.106 6-0.301 7 mg·mL-1(r=0.999 3), 0.100 2-0.300 6 mg·mL-1(r=0.998 5), 0.250 1-5.001 6 mg·mL-1(r=1.000) and 0.080 8-2.423 3 mg·mL-1(r=0.999 3), respectively. The average recoveries were 107.4%(RSD=1.1%),106.9%(RSD=1.5%),100.4%(RSD=1.2%),109.1%(RSD=1.9%),101.8%(RSD=1.6%),103.8%(RSD=5.2%) and 104.1%(RSD=0.50%), respectively. The contents of acetaldehyde, butyraldehyde, crotonaldehyde, tert-butanol, 2-ethylbutyl alcohol, 2-ethylbutyric acid and paraldehyde in 3 batches were 0.02%-0.31%,0.57%-1.0%,0.01%-0.02%,0.24%-0.33%, not detected-0.25%,2.2%-3.9%and 0.66%-1.9%, respectively. Conclusion: With good resolution and accuracy, the method can be reliably and effectively used in the determination of seven impurities in 2-ethylbutanal as well as provides a guarantee for the quality control of 2-ethylbutanal.
PAN Xian-wei, CHEN Si-qin, YU Jia-yan
. Determination of seven impurities in 2-ethylbutanal[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(5)
: 838
-844
.
DOI: 10.16155/j.0254-1793.2022.05.13
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