尿中丙酮的自动顶空-大口径毛细管柱气相色谱测定法  

Determination of acetone in urine by automatic headspace-large caliber capillary column gas chromatography

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作  者:赵好[1] 嵇童童 查河霞[1] 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)

机构地区:[1]南京市疾病预防控制中心理化检验科,江苏210003

出  处:《环境与健康杂志》2023年第4期349-351,共3页Journal of Environment and Health

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.

关 键 词:尿 丙酮 大口径毛细管柱 自动顶空 色谱法 气相 

分 类 号:O657.6[理学—分析化学]

 

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