首页|同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定法

同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定法

扫码查看
目的 建立同时测定尿中反-反式黏糠酸和苯巯基尿酸的在线固相萃取-液相色谱-质谱测定方法.方法 尿样离心后上机,经在线固相萃取HLB柱(20 mm×3.9 mm×15 μm)净化、富集,经C18柱(150 mm×4.6 mm×5 μm)分析,线性离子阱质谱检测.结果 反-反式黏糠酸和苯巯基尿酸的线性范围为0.0~15.0 mg/L、0.0~500.0 µg/L,相关系数为0.999 8、0.999 9,检出限为3.5、0.1 µg/L,样品加标回收率为103.3%~108.8%,相对标准偏差为2.8%~8.4%.结论 该方法样品前处理只需离心,操作简便快捷、结果准确、重现性好、灵敏高,适用于大批量的苯职业接触人群生物监测指标的检测.
Simultaneous determination of trans-trans mucofuric acid and phenylthiouric acid in urine by online solid-phase extraction liquid chromatography mass spectrometry
Objective To establish an online solid-phase extraction liquid chromatography-mass spectrometry method for the simultaneous determination of trans-trans mucofuric acid and phenylmercaptouric acid in urine.Methods The urine samples were centrifuged and processed on the machine,purified and enriched by online solid-phase extraction on HLB column(20 mm×3.9 mm×15 μm),and analysed by C18 column(150 mm×4.6 mm×5 μm),detec ted by linear ion trap mass spectrometry.Results The linear range of trans-trans mucofuric acid and phenylmercaptouric acid were 0.0-15.0 mg/L and 0.0-500.0 μg/L,with correlation coefficients of 0.999 8 and 0.999 9,and detection limits of 3.5 and 0.1 μg/L,the recovery rates were 103.3% -108.8% ,and the relative standard deviations were 2.8% -8.4% .Conclusion The sample pre-treatment of this method only requires centrifuged,which is simple and fast,with accurate results,good reproducibility and high sensitivity,and it was suitable for the detection of biological monitoring indicators in large quantities of occupational benzene exposure population.

Online solid-phase extractionLiquid chromatography-mass spectrometryUrineTrans-trans mucofuric acidPhenylmercaptouric acidBenzene metabolites

何宗剑、莫玉茗、宁攀良、朱定姬、覃利梅、李燕

展开 >

广西壮族自治区职业病防治研究院理化检测所,广西南宁 530021

广西医科大学公共卫生学院,广西南宁 530021

在线固相萃取 液相色谱-质谱法 尿 反反-粘糠酸 苯巯基尿酸 苯代谢物

广西壮族自治区卫生健康委员会课题

Z-A20230412

2024

职业与健康
天津市疾病预防控制中心 中华预防医学会

职业与健康

CSTPCD
影响因子:0.737
ISSN:1004-1257
年,卷(期):2024.40(13)
  • 15