摘要
目的建立尿中高香草酸和香草扁桃酸测定的高效液相色谱-串联质谱（HPLC／MS／MS）法。方法取尿样200μl置于离心管中，分别加入20μl氯唑沙宗内标，混匀后加入100μl甲醇（含1％乙酸），涡旋震荡1min，13000r／min（半径8．2cm）离心5min，提取上清后，取10μl进样，利用HPLC／MS／MS法对高香草酸和香草扁桃酸进行定性定量分析。结果该方法测定高香草酸和香草扁桃酸的线性范围分别为20．10000和20～7500ng／ml，相关系数分别为0．9956和0．9970，检出限分别为4．69和2．33ng／m1，回收率分别为85．72％。117．95％和95．82％-113．78％。结论该方法操作简便、快速、准确、灵敏度高，可满足尿中高香草酸和香草扁桃酸测定的要求。
Objective To establish a method for the determination of homovanillie acid （HVA） and vanil mandelic acid （VMA） in urine, using high performance liquid chromatography-tandem mass spectrometry （HPLC/MS/MS）detection. Methods A 200 μl volume of urine sample added with 20 μl chlorzoxazone internal standard was mixed in a centrifuge tube, then added 100μL methanol （containing 1% acetic acid）, vortex mixed and centrifuged at 13 000 rpm for 1 min. A 10 μl volume of the above supernatant solution was injected into HPLC/MS/MS system for quantitative analysis. Results With internal standard method, the calibration curves of HVA and VMA were linear in the range of 20-10 000 ng/ml and 20-7 500 ng/ml, with correlation coefficient of 0.995 6 and 0.997 0, respectively. The LOQ of HVA and VMA was 4.69 ng/ml and 2.33 ng/ml, respectively. The method recoveries were in the range of 85.72%-117.95% for HVA, and 95.82%-113.78% for VMA. Conclusion This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of homovanillic acid and vanilla mandelic acid.
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
2016年第6期461-465,共5页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
北京市自然科学基金资助项目（7142064）
关键词
色谱法
高压液相
尿
高香草酸
香草扁桃酸
Chromatography, high pressure liquid
Urine
Homovanillic acid
Vanil mandelic acid
