Determination of Benzene Residue in Alanyl Glutamine API by Headspace Gas Chromatography
Establish a headspace gas chromatography method for detecting petroleum ether residue in Alanyl Glutamine API.Method:A capillary column with 6%cyanopropyl benzene and 94%dimethyl siloxane as the stationary phase(Agilent DB-624 30.0 m*0.250 mm,1.40 μm,or similar polarity)was used as the chromatographic column.The initial column temperature is 70℃,maintained for 2 minutes,increased to 120℃at a rate of 10℃per minute,and then increased to 220℃at a rate of 20℃per minute,maintained for 3 minutes.The equilibrium temperature of the headspace bottle is 80℃,the equilibrium time is 20 minutes,and the detector is FID,with a detector temperature of 250℃;The temperature of the injection port is 200℃.Result:Using this method,the blank solvent has no interference,high sensitivity,linear regression equation is y=396 903.576x+559.762(n=6),correlation coefficient(r)0.999 8,recovery rate between 90.90%and 99.93%,RSD of 9 determination results is 3.3%,specificity,precision,and durability are all good,and the solution is stable within 24 hours,both meets the requirements of analytical method validation.This method was proved to be simple,repeatable,and suitable for the determination of benzene residue in Alanyl Glutamine API.
gas chromatographyheadspaceAlanyl Glutamine APIbenzene residue
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