Determination of Residual Organic Solvents in α-Ketovaline Calcium Raw Material by Headspace Capillary Gas Chromatography

OBJECTIVE: To establish a method for the content determination of residual organic solvents in α-ketovaline calcium, such as alcohol, ethyl ether, acetone, and ethyl acetate. METHODS: Headspace gas chromatography was adopted. Residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃, the inlet temperature was 150 ℃ with water as the solvent. RESULTS: The linear ranges of alcohol, ethyl ether, acetone and ethyl acetate all were 0.01～2.0 mg·mL-1 (r=0.999 9). The average recoveries were 98.6%～99.7% (RSD=1.0%～1.5%).The determination limits were 0.51～5.04 μg·mL-1. The residual levels of 4 kinds of organic solvents in 3 batches of samples were all up to the standard stated in Chinese Pharmacopeia. CONCLUSION: The method is simple, accurate, sensitive and reproducible. It can be used for the determination of the residual organic solvents in α-ketovaline calcium.