Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Highway NE, Mailstop F17, Atlanta, GA 30341, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Apr 15;878(13-14):957-62. doi: 10.1016/j.jchromb.2010.02.025. Epub 2010 Mar 1.
We report an improved solid-phase extraction-high-performance liquid chromatography-tandem mass spectrometry method with isotope dilution quantification to measure seven atrazine metabolites in urine. The metabolites measured were hydroxyatrazine (HA), diaminochloroatrazine (DACT), desisopropylatrazine (DIA), desethylatrazine (DEA), desethylatrazine mercapturate (DEAM), atrazine mercapturate (ATZM), and atrazine (ATZ). Using offline mixed-mode reversed-phase/cation-exchange solid-phase extraction dramatically increased recovery and sensitivity by reducing the influence of matrix components during separation and analysis. DACT extraction recovery improved to greater than 80% while the other analytes had similar extraction efficiencies as previously observed. Limits of detection were lower than our previous method (0.05-0.19 ng/mL) with relative standard deviations less than 10%. The total runtime was shorter (18 min) than the previous on-line method, thus it is suitable for large-scale sample analyses. We increased the throughput of our method twofold by using the newer extraction technique.
我们报道了一种改进的固相萃取-高效液相色谱-串联质谱法,采用同位素稀释定量法测定尿液中的七种莠去津代谢物。所测定的代谢物有羟基莠去津(HA)、二氨基氯莠去津(DACT)、去异丙基莠去津(DIA)、去乙基莠去津(DEA)、去乙基莠去津巯基尿酸(DEAM)、莠去津巯基尿酸(ATZM)和莠去津(ATZ)。采用离线混合模式反相/阳离子交换固相萃取,通过减少分离和分析过程中基质成分的影响,显著提高了回收率和灵敏度。DACT 的提取回收率提高到 80%以上,而其他分析物的提取效率与之前观察到的相似。检测限低于我们之前的方法(0.05-0.19ng/mL),相对标准偏差小于 10%。总运行时间(18 分钟)比之前的在线方法更短,因此更适合大规模样品分析。我们通过使用新的提取技术将方法的通量提高了两倍。