[Determination of the butanone in urine by gas chromatography with precolumn derivation]

Objective: To establish a method for determination of the butanone in urine by gas chromatography (GC) with pre-column derivation. Methods: For detecting of butanone in urine, potassium iodide and potassium dichromate were added into urine under acidic condition, sample derivatization was undertaken in 50 ℃ water bath for 60 min and the iodine butanone was extracted with n-hexane. After the sodium thiosulfate solution was used to remove excess iodine, urine samples were centrifuged at 10000 r/min for 5 min, then the supernatant was analyzed using temperature rising programming with the Agilent Hp-5 column (30 m×0.32 mm, 0.25 μm) and electron capture detector (ECD) as the detector. The detector temperature was 300 ℃, the inlet temperature was 200 ℃, and the carrier gas was nitrogen. Results: For detecting of butanone in urine, potassium iodide and potassium dichromate were added for derivatization under the acidic condition. After extraction and centrifugation, the supernatant directly put through column and detected by ECD. In present study, the sample pretreatment condition was optimized, the relative standard deviations of intra-day and inner-day, the spiked samples and its recovery were evaluated for analyzing the accuracy of the proposed method. Conclusion: This method has proved to be simple, efficient and highly sensitivity, it can be utilized for butanone detection in occupational population.