尿中丁二烯代谢产物的生物检测方法  

Biological determination method of butadiene metabolites in human urine

作　　者：李仁波[1] 赵敬[2] 高衍新[1] 夏昭林[3] 程学美[1] LI Ren- bo ZHAO Jing GAO Yan- xin XIA Zhao -lin CHENG Xue -mei(Shandong Center for Disease Control and Prevention, Ji＇nan, Shandong 250014, China)

机构地区：[1]山东省疾病预防控制中心,山东济南250014 [2]山东省职业卫生与职业病防治研究院,山东济南250062 [3]复旦大学,上海200032

出　　处：《中国卫生检验杂志》2017年第10期1369-1371,1374,共4页Chinese Journal of Health Laboratory Technology

基　　金：国家职业卫生标准项目(20130202);山东省自然科学基金-青年基金项目资助(ZR2010HQ042);山东省医药卫生研究项目(2009HZ050);山东省科技发展计划项目(2015WS0275)

摘　　要：目的研究尿中丁二烯代谢产物1,2-双羟基-4-(N-乙酰半胱氨酸)-丁烷(DHBMA)和1-(N-乙酰半胱氨酸)-2-羟基-3-丁烯(MHBMA)的超高效液相色谱-质谱/质谱(UPLC-ESI-MS/MS)测定方法,对丁二烯暴露工人进行生物监测。方法尿液经1∶10稀释[100μl尿样+50μl混合内标应用液+850μl流动相A(15 mmol/L乙酸铵,p H=6.8)],涡旋混匀,过膜后直接进样,UPLC-ESI-MS/MS测定,工作曲线内标法定量。结果 DHBMA的定量检出限为0.50μg/L,尿中最低检出质量浓度为5.0μg/L,线性相关系数>0.996,高、中、低浓度加标回收率为93%~106%;MHBMA的定量检出限为0.07μg/L,尿中最低检出质量浓度为0.70μg/L,线性相关系数>0.998,高、中、低浓度加标回收率为84%~106%。结论 UPLC-ESI-MS/MS法测定丁二烯代谢产物DHBMA和MHBMA浓度的各项技术指标均能满足生物样品监测的要求,可用于职业场所工作人员的生物监测。Objective To study the ultra performance liquid chromatography tandem mass spectrometric （UPLC -ESI -MS/MS） method for simultaneous determination of the metabolites of 1,3 - butadiene, 1,2 - dihydroxy -4 - N - acetyl - 1 - cysteine - butyl （DHBMA） and 1 - N - acetyl - 1 - cysteine - hydroxy - 3 - butene （MHBMA）. Methods The urine sample was diluted 10 times [ 100μl the urine sample ＋ 50 μl mixed internal standard application ＋ 850μl mobile phase A （ 15 mmol/L ammonium acetate, pH ：6.8）], vortex mixed, filtered through membrane, then detected by UPLC -ESI- MS/MS system with standard working curve method and internal standard method for quantification. Results The quantitative detection limit of DHBMA was 0.50μg/L, and the lowest detection of urine DHBMA concentration was 5.0 μg/L, and correlation coefficient of the method was greater than 0. 996. The recovery rate at high, median and low concentration was from 93% to 106%. The quantitative de- tection limit of MHBMA was 0.07 μg/L, and the lowest detection of urine MHBMA concentration was 0.70 μg/L, and the cor- relation coefficient of the method was greater than 0. 998. The recovery rate at high, median and low concentration was from 84% to 106%. Conclusion The method for urinary DHBMA and MHBMA concentration determination with UPLC - ESI - MS/MS can meet the requirements of biological sample monitoring and be used for the biological monitoring of oeeupational workers.

关 键 词：1 3-丁二烯 生物检测方法 超高效液相色谱-质谱/质谱 

分 类 号：R446.1[医药卫生—诊断学]