气相色谱-质谱联用法测定人尿中的沙丁胺醇

Determination of Salbutamol in Human Urine by GC -MS

目的:建立人尿中沙丁胺醇测定的GC-MS方法。方法:酶解后的尿样经pH 9.5的氯化铵缓冲液碱化后,过Bond Elut-Certify小柱,用氯仿-异丙醇(4:1)+2%氨水提取,提取液吹干后用MSTFA进行硅烷化,采用GC-EI-MS法,选择离子方式检测。结果:人尿中沙丁胺醇检测的线性范围为4.0-2000.0 ng·mL-1,最低检测限可达0.7 ng·mL-1。人尿中沙丁胺醇的提取回收率为69.3%-72.4%,日内RSD和日间RSD均不大于7.24%。结论:本方法灵敏、准确,可用于运动员尿样的兴奋剂检测。

Objective:To develop a gas chromatography - mass spectrometry( GC-MS) method for the determina tion of salbutamol in human urine. Methods:The urine after enzymatic hydrolysis was alkalized with pH 9. 5 ammonium chloride buffer solution and was extracted by Bond Elut - Certify cartridges, salbutamol was eluted by a solution consisted of chloroform - isopropyl alcohol(4:1)+2% a mmonia. The extracted solution was dried by nitrogen flow and silylanized by MSTFA. The analytes were detected by electric ionization(EI)-MS method under selected - ion monitoring( SIM) mode. Results:The linear range of the urine concentration of salbutamol was 4. 0 - 2000. 0 ng·mL-1 ,and the limited of detection was 0. 7 ng ·mL-1. The extracted recoveries of salbutamol were 69. 3% -72. 4% . The intra - day RSD and inter - day RSD were both less than 7. 24%. Conclusion: The method has high sensitivity and good selectivity, it can be used for the urinary detection of doping agent.