摘要
目的建立和完善高效液相色谱-离子阱质谱联用检测尿苯中巯基尿酸(S-PMA)的方法。方法样品通过液-液萃取技术提取后进入Agilent Extend C18色谱柱,流动相为乙酸铵和甲醇的混合物,采用梯度洗脱的方式实现样品的分离。以ESI模式进行质谱数据采集,对所得谱图进行分析。结果本方法线性回归方程为A=90.2488c+3896.3869,回归系数r=0.9995,线性范围为10～5000μg/L,检出限为10μg/L,灵敏度为0.0011μg/L,样品回收率77.8%～81.4%,相对标准偏差RSD为0.9%～1.2%,精密度日内误差为0.9%～1.2%,日间误差为0.9%～1.7%。结论本研究建立的尿S-PMA高效液相色谱-离子阱质谱联用方法,简捷快速、结果准确,为职业卫生工作中尿S-PMA的日常常规检测奠定了基础。
Objective To establish and improve the liquid chromatographic/mass spectrometry methods for urinary S- phenylmercapturic acid（S- PMA）. Methods Urine samples were acidified and then purified liquid-liquid extraction. Analyses were conducted on a Agilent Extend C18 chromatographic column by gradient elution with acetic acid/methanol mixtures at different proportions as the mobile phase. The detector was used in electrospray negative ion mode （ESI-） to obtained the chromatogram and mass spectrograph. Result The typical calibration curves was A = 90. 2488c ＋ 3896. 3869 with r = 0. 9995. The detection limit was 10μg/L, the sensibility was 0. 0011, the recovery rate was from 77.8 % to 81.4 %, the intra - day standard deviation was from 0.9 % to 1.2 % and the inter - day standard deviation was from 0.9 % to 1.7 %. Conclusion This liquid chromatographic/ mass spectrometry methods for urinary S- PMA had conciser procedure and accurate outcome and was possible to be take as a routine method in the occupational health.
出处
《实用预防医学》
CAS
2007年第4期1009-1012,共4页
Practical Preventive Medicine
基金
广州市科技攻关项目(2005Z3-E0131)
关键词
苯巯基尿酸
高效液相色谱法
质谱法
联用技术
S - phenylmercapturic acid
High efficiency liquid chromatography
Mass spectrography
Multiple techniques
