Determination of Piperidine and Pyridine in Tydiloxine by Head-space Gas Chromatography
A head-space gas chromatography method was established to determine the content of piperidine and pyridine in Tydiloxine.A Rtx-35 Amine column(30 m×0.32 mm,1 μm)with a stationary liquid of 35％biphenyl-65％dimethyl polysiloxane and a hydrogen flame ionization detection were used.Column temperature was programmed with an injector temperature of 220 ℃ and a detector temperature of 250 ℃.The carrier gas was high-purity nitrogen with a flow rate of 1.5 mL/min.The headspace equilibration temperature was set at 90 ℃,and the equilibration time was 30 minutes.The separation factor between pyridine and piperidine was greater than 2.0,and there was no interference from the blank solvent.Pyridine and piperidine showed good linear relationships within their respective concentration ranges(r≥0.999 8).The detection limits of pyridine and piperidine were 0.13 μg/mL and 0.12 μg/mL,and the quantification limits were 0.41 μg/mL and 0.40 μg/mL,respectively.The average recovery rates for impurities were 101.7％and 102.2％,respectively.This method possessed strong specificity,high sensitivity,and good accuracy,meeting the requirements for the determination of the content of piperidine and pyridine in Tydiloxine.
head-space gas chromatographytydiloxinepyridinepiperidinecontent
万方数据
维普
