Abstract:
OBJECTIVE To establish a method for the determination of 12 residual organic solvents in glycine as methanol, alcohol, acetone, isopropyl alcohol, acetonitrile, dichloromethane,
N-propanol, ethyl acetate, tetrahydrofuran, cyclohexane,
N-butyl alcohol, and toluene.
METHODS Headspace GC was adopted. The determination was performed on DB-624 capillary column (30 m×0.53 mm, 3.0 μm) using temperature programming with FID. The inlet temperature was 150℃, and flame ionization detector was used with temperature of 250℃. High purity nitrogen was used as carrier gas with flow rate of 2.2 mL·min
-1. The split ratio was 10:1. Headspace heating temperature was 80℃, and equilibration time was 35 min.
RESULTS There was good linear relationship in the concentration ranges of 12 residual organic solvents with correlation coefficient above 0.999, respectively. RSDs of precision and stability tests were all <5%, and alcohol, acetone and isopropyl alcohol were found in repeatability test (RSD ≤ 1.8%). The average recoveries were within 97%-102%.
CONCLUSION The established method is simple, accurate and reproducible, and can be used for simultaneous determination of 12 residual organic solvents in the raw material of glycine.