人尿中9种单羟基多环芳烃的固相萃取-超高效液相色谱-串联质谱同时测定法

发布时间：2018-03-23 03:21

本文选题：固相萃取-超高效液相色谱-串联质谱　切入点：尿　出处：《环境与健康杂志》2017年03期 　论文类型：期刊论文

【摘要】：目的建立同时测定尿中9种单羟基多环芳烃(OH-PAHs,即1-羟基萘、2-羟基萘、3-羟基芴、3-羟基菲、1-羟基芘、3-羟基■、6-羟基■、3-羟基苯并蒽和9-羟基苯并芘)的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)法。方法将10 ml尿样经酶水解、C18固相萃取柱(500 mg,3 ml)提取富集后,用Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1×100 mm,1.7μm)分离,在三重四级杆串联质谱负离子模式下检测,以内标法定量分析。结果尿中9种目标化合物在0.102~40 ng/ml范围内均呈良好的线性关系(r0.999),检出限(S/N=3)为0.01~0.32 ng/ml,样品在1.6、4.0、10 ng/ml浓度水平的平均加标回收率为91.5%~128%,相对标准偏差(RSD)15%。结论该方法用时短,灵敏度高,准确度好,精密度高,适合人群尿中多环芳烃代谢物的监测。
[Abstract]:Objective to establish a method for simultaneous determination of nine monohydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine, I. e. 1-hydroxy-naphthalene 2-hydroxy-naphthalene 3-hydroxyfluorene 3-hydroxy-1-hydroxy-pyrene 3-hydroxy-6-hydroxy-6-hydroxy-3-hydroxybenzo-anthracene and 9- hydroxy benzo (pyrene). High performance liquid chromatography-tandem mass spectrometry SPE-UPLC-MS / MS.Methods 10ml urine samples were extracted and enriched by enzymatic hydrolysis of C18 solid phase extraction column (500mg / 3ml). Waters ACQUITY UPLC BEH Che _ (18) chromatographic column (2.1 脳 100mm ~ (-1) 渭 m) was used for detection of anion in tandem mass spectrometry. Results there was a good linear relationship between the nine target compounds in urine in the range of 0.102 ~ 40 ng/ml. The detection limit (S / N ~ (3)) was 0.01 ~ 0.32 ng / ml. The average recoveries of the samples at the concentration level of 1.66 ~ 4.0 ~ (10) ng/ml were 91.5128 and the relative standard deviation was 15 ~ 15ng-1 / ml. On the short time of this method, High sensitivity, high accuracy and high precision. It is suitable for monitoring the metabolites of polycyclic aromatic hydrocarbons (PAHs) in human urine.
【作者单位】：中国疾病预防控制中心环境与健康相关产品安全所;中国疾病预防控制中心研究生院;
【基金】：环境保护部国家环保公益性行业科研专项(201309045)
【分类号】：O657.63;R446.12

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