Determination of diisopropylamide dichloroacetate concentrations in urine by GC-HS / 重庆医科大学学报

ABSTRACT

Objective:To establish a method for determination of diisopropylamide dichloroacetate(DADA) concentrations in urine.Methods:GC-HS was applied to quantitative analysis.Using Agilent DB-5MS capillary column(30m?0.25mm),the column temperature was ascended from 40℃ to 200℃ according to program.Initial temperature was 40℃ and maintained 2 mins,then temperature rose to 80℃ at 5℃/min rate and maintained 2 mins,finally temperature rose to 200℃ at 20℃/min rate and maintained 8 mins.The injector temperature was 200℃.The detector temperature was 300℃.Nitrogen was used as carrier gas,and the flow rate was 1 ml/min.The flow rate of hydrogen was 35 ml/min.The flow rate of air was 350 ml/min.An internal standard was secondary butanol.Results:The calibration curve was linear within 8～800?g/ml.The recovery rate of the extraction were 88.75%～98.06%.The recovery rate were 97.36%～103.25%。Within-day and between-day RSD were 2.95%～6.62% and 2.45%～5.61% respectively.Detectable concentration limited was 2?g/mL.Conclusion:The GC-HS method is simple,reliable,and suitable for urine DADA concentration analysis.