中华劳动卫生职业病杂志
中華勞動衛生職業病雜誌
중화노동위생직업병잡지
CHINESE JOURNAL OF INDUSTRIAL HYGIENE AND OCCUPATIONAL DISEASES
2014年
2期
142-144
,共3页
反-反式黏糠酸%苯巯基尿酸%8-羟基脱氧尿苷%色谱法,液相色谱-质谱
反-反式黏糠痠%苯巰基尿痠%8-羥基脫氧尿苷%色譜法,液相色譜-質譜
반-반식점강산%분구기뇨산%8-간기탈양뇨감%색보법,액상색보-질보
8-Hydroxy-2'-deoxyguanosine%Trans,trans-muconic acid%S-phenylmercapturic acid%Chromatography%Liquid chromatography-mass spectrometry
目的 建立苯作业工人尿中3种生物标志物8-羟基脱氧尿苷、反-反式黏糠酸和苯巯基尿酸同时测定的方法.方法 尿样经固相萃取柱净化后,用液相色谱-质谱仪进行测定,用外标法定量,色谱柱采用C18反相色谱柱,流动相为甲醇与酸性甲酸铵溶液梯度淋洗,质谱采集方式为多反应监测.结果 反-反式粘糠酸测定的线性范围为10～1000μg/L,当添加浓度为50μg/L和500μg/L时,回收率均大于90％,相对标准偏差小于3％；苯巯基尿酸与8-羟基脱氧尿苷测定的线性范围为1～100 μg/L,当添加浓度为5μg/L和50μg/L时,回收率均大于85％,相对标准偏差小于5％.结论 本检测方法各项指标均符合WS/T 68-1996《研制生物样品监测检验方法指南》的要求,适用于尿中苯的3种生物标志物的同时测定.
目的 建立苯作業工人尿中3種生物標誌物8-羥基脫氧尿苷、反-反式黏糠痠和苯巰基尿痠同時測定的方法.方法 尿樣經固相萃取柱淨化後,用液相色譜-質譜儀進行測定,用外標法定量,色譜柱採用C18反相色譜柱,流動相為甲醇與痠性甲痠銨溶液梯度淋洗,質譜採集方式為多反應鑑測.結果 反-反式粘糠痠測定的線性範圍為10～1000μg/L,噹添加濃度為50μg/L和500μg/L時,迴收率均大于90％,相對標準偏差小于3％；苯巰基尿痠與8-羥基脫氧尿苷測定的線性範圍為1～100 μg/L,噹添加濃度為5μg/L和50μg/L時,迴收率均大于85％,相對標準偏差小于5％.結論 本檢測方法各項指標均符閤WS/T 68-1996《研製生物樣品鑑測檢驗方法指南》的要求,適用于尿中苯的3種生物標誌物的同時測定.
목적 건립분작업공인뇨중3충생물표지물8-간기탈양뇨감、반-반식점강산화분구기뇨산동시측정적방법.방법 뇨양경고상췌취주정화후,용액상색보-질보의진행측정,용외표법정량,색보주채용C18반상색보주,류동상위갑순여산성갑산안용액제도림세,질보채집방식위다반응감측.결과 반-반식점강산측정적선성범위위10～1000μg/L,당첨가농도위50μg/L화500μg/L시,회수솔균대우90％,상대표준편차소우3％；분구기뇨산여8-간기탈양뇨감측정적선성범위위1～100 μg/L,당첨가농도위5μg/L화50μg/L시,회수솔균대우85％,상대표준편차소우5％.결론 본검측방법각항지표균부합WS/T 68-1996《연제생물양품감측검험방법지남》적요구,괄용우뇨중분적3충생물표지물적동시측정.
Objective To establish a method for simultaneously determining the urinary concentrations of 8-hydroxy-2'-deoxyguanosine (8-OHdG),trans,trans-muconic acid (tt-MA),and S-phenylmercapturic acid (S-PMA) in subjects exposed to benzene.Methods After being purified by a solid-phase extraction column,the urine samples were transferred to a liquid chromatography-mass spectrometry system,and the concentrations of 8-OHdG,tt-MA,and S-PMA were determined by external standard method.A C18 reversed-phase column was used as the chromatographic column,and methanol/acidic ammonium formate solution was used as the mobile phase for gradient elution.The mass spectrometer was operated in a multi-reaction monitoring mode.Results For tt-MA,the calibration curves were linear in the range of 10-1000 μg/L,and the recovery rates were over 90％ (relative standard deviation (RSD) ＜3％) at spiked levels of 50 μg/L and 500 μg/L.For S-PMA and 8-OHdG,the calibration curves were linear in the range of 1-100 μg/L,and the recovery rates were over 85％ (RSD ＜5％) at spiked levels of 5 μg/L and 50 μg/L.Conclusion This determination method meets the requirement of Biological materials-Methods of monitoring-Guide of development (WS/T 68-1996) and can be used for simultaneous determination of 8-OHdG,tt-MA,and S-PMA in urine.
