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固相支撑液液萃取结合超高效液相色谱-串联质谱法同时测定尿液中7种多环芳烃代谢物
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作者单位
陈雪蕾,李冬梅,徐厚君,王学生,王曼曼 1.华北理工大学公共卫生学院2.华北理工大学药学院 
基金项目:国家自然科学基金项目(21305028);河北省自然科学基金项目(H2017209232,H2016209018);河北省教育厅重点项目(ZD2018014);华北理工大学培育基金项目(JQ201717)
中文摘要:建立了固相支撑液液萃取法(SLE)结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定尿液中1-羟基萘、2-羟基萘、2-羟基芴、9-羟基芴、2-羟基菲、9-羟基菲和1-羟基芘7种羟基多环芳烃(OH-PAHs)的方法。实验将0.8 mL尿液酶解液经SLE萃取,考察了洗脱溶剂种类及体积的影响,并对氮吹浓缩压力进行了优化。尿液样品使用6 mL乙酸乙酯洗脱,洗脱液在48 kPa(25 ℃)压力下氮吹至干后,经UPLC-MS/MS对7种OH-PAHs进行分析,采用同位素内标法定量。方法在0.3~3 000 mg·L-1范围内线性关系良好(r≥0.995 1),检出限和定量下限分别为0.05~1.0 mg·L-1和0.15~3.0 mg·L-1。加标3个浓度水平的回收率为70.8%~117%,日内(n=3)和日间(n=3)相对标准偏差分别为3.7%~9.6%和3.7%~11%。采用本方法对10例石油工人和10例对照人群(在校大学生)尿液中的OH-PAHs水平进行分析,除2-羟基菲和9-羟基菲外,其余5种OH-PAHs在石油工人尿液中的含量均高于对照人群(p<0.05),差异具有统计学意义。该方法经上样和洗脱两步完成样品前处理,简单高效,可用于尿液样品中OH-PAHs的分析。
中文关键词:羟基多环芳烃(OH-PAHs)  固相支撑液液萃取法(SLE)  超高效液相色谱-质谱法(UPLC-MS/MS)  尿液
 
Simultaneous Determination of 7 Hydroxyl Polycyclic Aromatic Hydrocarbons in Urine by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Supported Liquid-Liquid Extraction
Abstract:An ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with solid supported liquid-liquid extraction(SLE) was developed for the determination of seven hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs) in urine samples.08 mL enzymatic hydrolyzed urine sample was extracted on a SLE cartridge.Parameters for SLE,including type and volume of eluting solvent,and nitrogen evaporation pressure were optimized.The adsorbed analytes were eluted with 6 mL ethyl acetate,and the collected eluate was evaporated to dryness under nitrogen at a pressure of 48 kPa at 25 ℃,then analyzed by UPLC-MS/MS and quantified by the internal standard method.Under the optimized conditions,the calibration curves for the analytes were linear in the range of 0.3-3 000 mg·L-1,with correlation coefficients not less than 0.995 1.The detection limits(S/N=3) and quantitation limits(S/N=10) were in the ranges of 0.05-1.0 mg·L-1 and 0.15-3.0 mg·L-1,respectively.The recoveries for OH-PAHs in urine samples at three spiked levels ranged from 70.8% to 117%,with the intra day(n=3) and inter-day(n=3) RSDs of 3.7%-9.6% and 3.7%-11%,respectively.The proposed method was successfully applied in the determination of OH-PAHs in urine from 10 petroleum workers and 10 control groups(college students).Except 2-hydroxy phenanthrene and 9-hydroxy-phenanthrene,the concentrations of the other five OH-PAHs in the urine samples of petroleum workers were much higher than that in the control samples(p<0.05).The proposed SLE method only included two steps,therefore,the proposed method is applicable for the facile and efficient monitoring of OH-PAHs in urine samples.
Key Words:hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs)  solid supported liquid-liquid extraction(SLE)  ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  urine
引用本文:陈雪蕾,李冬梅,徐厚君,王学生,王曼曼.固相支撑液液萃取结合超高效液相色谱-串联质谱法同时测定尿液中7种多环芳烃代谢物[J].分析测试学报,2019,(3):270-276.
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