超高效液相色谱串联质谱检测生物样本中多环芳烃  

An ultrasensitive UPLC-MS-MS method for the analysis of carcinogenic polycyclic aromatic hydrocarbons in human samples

作　　者：李欣欣[1,2] 崔师伟[1] 何民富[3] 杨功焕[4] 孙新[1] 

机构地区：[1]中国疾病预防控制中心化学安全与健康重点实验室,中国疾病预防控制中心职业卫生与中毒控制所,北京100050 [2]北京市大兴区疾病预防控制中心 [3]中国疾病预防控制中心慢性非传染性疾病预防控制中心 [4]中国疾病预防控制中心

出　　处：《中国预防医学杂志》2012年第4期246-250,共5页Chinese Preventive Medicine

基　　金：国家高技术研究发展计划(863)(No.2008AA062504)

摘　　要：目的建立高灵敏度的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,用于检测生物样本中痕量多环芳烃(PAHs),包括血浆中3种致癌性多环芳烃苯并(a)芘(BaP)、苯并(g,h,i)苝[B(g,h,i)P]、二苯并(a,h)蒽[DB(a,h)A],及尿液中三种羟基多环芳烃代谢产物2-羟基萘(2-OHN)、2-羟基芴(2-OHF)、1-羟基芘(1-OHP)。方法血浆经饱和氯化钠过夜盐析,尿液经β-葡糖苷酸酶水解,固相萃取后,用UPLC-MS/MS分析。结果血浆中3种致癌性多环芳烃在0.5～100μg/L浓度范围内呈良好的线性关系,线性相关系数均大于0.99,加标回收率为87%～124%,日内精密度为0.91%～10.31%,日间精密度为4.59%～15.83%,血浆中3种致癌性多环芳烃BaP、B(g,h,i)P、DB(a,h)A的检出限分别为0.33、0.41和0.65μg/L;尿液中3种羟基多环芳烃代谢产物在0.5～100μg/L浓度范围内呈良好的线性关系,线性相关系数均大于0.99,加标回收率为81.8%～110.5%,日内精密度为1.28%～8.56%,日间精密度为6.87%～10.91%,尿液中3种羟基多环芳烃代谢产物2-OHN、2-OHF、1-OHP的检出限分别为0.17、0.03和0.04μg/L。结论该方法生物样本用量少,回收率较高,重现性好,检出限低,适用于人群多环芳烃的生物监测。Objective To develop a ultrasensitive performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） for simultaneous quantification of 3 carcinogenic PAHs in human plasma and 3 PAH metabolites in human urine.Methods Plasma PAHs and urinary PAH metabolites were enriched and separated by a solid-phase extraction,and were analyzed by UPLC-MS/MS.Results The substrate concentration-dependent response curve of PAHs in plasma by analyzing with UPLC-MS-MS showed a linear relation,ranging from 0.5 to 100 μg/L,the recovery of PAHs in plasma ranged from 87% to 124%.It was estimated that the limits of detection of BaP、B（g,h,i）P、DB（a,h）A in plasma were 0.33,0.41 and 0.65 μg/L,respectively;the substrate concentration-dependent response curve of urinary PAH metabolites by analyzing with UPLC-MS-MS was showed a linear relation,ranging from 0.5 to 100 μg/L,the recovery of urinary PAH metabolites ranged from 81.8% to 110.5%.It was estimated that the limits of detection for 2-OHN,2-OHF,1-OHP were 0.17、0.03 and 0.04 μg/L,respectively.Conclusions Our Non-invasive detection methods appear to be superior in terms of overall specificity and sensitivity,and could be explored as biomarkers for biomonitoring of PAHs.

关 键 词：多环芳烃 超高效液相色谱-串联质谱 检测方法 生物监测 

分 类 号：R114[医药卫生—卫生毒理学]