摘要
目的 建立尿中丙酮的自动顶空-大口径毛细管柱气相色谱测定方法。方法 向20 ml顶空瓶中依次加入2.0 g氯化钠和3.0 ml尿样,密封放入自动顶空仪80℃加热平衡30 min后,在分流比1∶1的条件下,经HP-INNOWAX色谱柱(30 m×0.530 mm,1.00μm)分离,氢火焰离子化检测器进行检测。结果 在0.05~157.6 mg/L范围内,所得尿中丙酮的回归方程为y=10.109 16x-10.380 56,r=0.999 3。该方法的检测限为0.01 mg/L,定量下限为0.05 mg/L;加标回收率为98%~103%,RSD为1.8%~4.0%。结论 该方法操作简单方便,灵敏度和准确度均较高,稳定性好,适合职业接触工人尿中丙酮的大批量测定。
Objective To establish an automatic headspace-large caliber capillary column gas chromatography method for the determination of acetone in urine.Methods 2.0 g of sodium chloride and 3.0 ml of urine sample were added into a 20 ml headspace bottle.The urine sample was immediately sealed and balanced in an automatic headspace at 80℃for 30 min.With the shunt ratio of 1∶1,the separation was performed on HP-INNOWAX(30 m×0.530 mm,1.00μm)chromatographic column,detected by FID.Results In the range of 0.05~157.6 mg/L,the regression equation of urine sample was y=10.10916x-10.38056,the correlation coefficient was 0.9993.The limit of detection was 0.01 mg/L,and the limit of quantification was 0.05 mg/L.The average recoveries were 98%-103%with relative standard deviations(RSD)of 1.8%-4.0%.Conclusion The automatic headspace gas chromatography has the advantages of accuracy,reliability,high sensitivity and simple operation,which can provide technical support for the detection of large quantities of health examination samples.
作者
赵好
嵇童童
查河霞
ZHAO Hao;JI Tong-tong;ZHA He-xia(Department of Physical and Chemical Analysis,Nanjing Center for Disease Control and Prevention,Nanjing,Jiangsu 210003,China)
出处
《环境与健康杂志》
北大核心
2023年第4期349-351,共3页
Journal of Environment and Health
关键词
尿
丙酮
大口径毛细管柱
自动顶空
色谱法
气相
Urine
Acetone
Large caliber capillary column
Automatic headspace
Chromatography,gas
