液液微萃取-高效液相色谱法快速测定尿液中的甲苯二胺
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摘要
目的建立尿液中甲苯二胺的液液微萃取-高效液相色谱测定方法。方法以塑料滴管为萃取容器,磷酸三丁酯为萃取剂,通过氢键相互作用对尿中甲苯二胺进行液液微萃取,萃取后的溶剂直接进样分析。结果在优化的萃取条件下,2,6-甲苯二胺与2,4-甲苯二胺在10.0～1 000μg/L范围内线性相关系数大于0.999,检出限分别为1.42μg/L和1.40μg/L,加标回收率分别为83.56%～105.1%和79.65%～104.9%,日内日间相对标准偏差均小于10%。结论本法操作简便,富集倍数高,前处理时间短,适用于职业接触甲苯二异氰酸酯人群尿中代谢产物甲苯二胺的测定。
Objective To establish a method for the determination of 2,4-diaminotoluene(2,4-DAT)and 2,6-diaminotoluene(2,6-DAT)in urine by liquid-liquid microextraction(LLME)combined with high performance liquid chromatography(HPLC).Methods Tributyl phosphate was used as an extractant for the pre-concentration of diaminotoluenes by hydrogen bonding interaction in a centrifuged device.The extractant was directly injected and analyzed by HPLC.Results Under the optimized conditions,the linearity range of the proposed method was 10.0-1 000 μg/L with correlation coefficients(r)greater than 0.999.The limits of detection for 2,4-DAT and 2,6-DAT were 1.42 μg/L and 1.40 μg/L,respectively.The recoveries were 83.56%～105.1% and 79.65%～104.9% with RSDs less than 10%.Conclusion This method is simple,sensitive and rapid for the determination of diaminotoluenes in urine for occupational population exposed to toluene diisocyanate.
Objective To establish a method for the determination of 2,4-diaminotoluene(2,4-DAT)and 2,6-diaminotoluene(2,6-DAT)in urine by liquid-liquid microextraction(LLME)combined with high performance liquid chromatography(HPLC).Methods Tributyl phosphate was used as an extractant for the pre-concentration of diaminotoluenes by hydrogen bonding interaction in a centrifuged device.The extractant was directly injected and analyzed by HPLC.Results Under the optimized conditions,the linearity range of the proposed method was 10.0-1 000 μg/L with correlation coefficients(r)greater than 0.999.The limits of detection for 2,4-DAT and 2,6-DAT were 1.42 μg/L and 1.40 μg/L,respectively.The recoveries were 83.56%～105.1% and 79.65%～104.9% with RSDs less than 10%.Conclusion This method is simple,sensitive and rapid for the determination of diaminotoluenes in urine for occupational population exposed to toluene diisocyanate.
引文
[1] 张雅萍,庞雅薇,刁望君.甲苯二异氰酸酯的生产和应用[J].氯碱工业,1999(1):38-40.
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[3] 季宇彬,汲晨锋,邹翔,等.气相质谱法对小鼠体内甲苯二异氰酸酯代谢产物的鉴定分析[J].光谱学与光谱分析,2007,27(9):1886-1889.
[4] 刘保峰,张明,封琳敏,等.甲苯二异氰酸酯职业接触人群尿中代谢产物调查[J].环境与健康杂志,2016,33(7):653-654.
[5] 张志涛,刘蕾,邵华.尿液中甲苯二异氰酸酯及其代谢产物的高效液相色谱法测定[J].化工管理,2015(9):91-92.
[6] Sakai T,Morita Y,Kim Y,et al.LC-MS determination of urinary toluenediamine in workers exposed to toluenediisocyanate[J].Toxicology Letters,2002,134(1/3):259-264.
[7] Sakai T,Morita Y,Roh J,et al.Improvement in the GC-MS method for determining urinary toluene-diamine and its application to the biological monitoring of workers exposed to toluene-diisocyanate[J].International Archives of Occupational and Environmental Health,2005,78(6):459-466.
[8] 黎关炼,顾缨缨,梅勇,等.分散液-液微萃取-高效液相色谱法测定尿中邻甲酚[J].现代预防医学,2018,45(14):2631-2634,2650.
[9] 胡西洲.新型样品前处理技术在环境和生物样品分析中的应用[D].武汉:武汉大学,2012.
[2] 巨睿,贾强,孟涛,等.甲苯二异氰酸酯职业接触对工人健康的影响[J].中华劳动卫生职业病杂志,2016,34(1):23-26.
[3] 季宇彬,汲晨锋,邹翔,等.气相质谱法对小鼠体内甲苯二异氰酸酯代谢产物的鉴定分析[J].光谱学与光谱分析,2007,27(9):1886-1889.
[4] 刘保峰,张明,封琳敏,等.甲苯二异氰酸酯职业接触人群尿中代谢产物调查[J].环境与健康杂志,2016,33(7):653-654.
[5] 张志涛,刘蕾,邵华.尿液中甲苯二异氰酸酯及其代谢产物的高效液相色谱法测定[J].化工管理,2015(9):91-92.
[6] Sakai T,Morita Y,Kim Y,et al.LC-MS determination of urinary toluenediamine in workers exposed to toluenediisocyanate[J].Toxicology Letters,2002,134(1/3):259-264.
[7] Sakai T,Morita Y,Roh J,et al.Improvement in the GC-MS method for determining urinary toluene-diamine and its application to the biological monitoring of workers exposed to toluene-diisocyanate[J].International Archives of Occupational and Environmental Health,2005,78(6):459-466.
[8] 黎关炼,顾缨缨,梅勇,等.分散液-液微萃取-高效液相色谱法测定尿中邻甲酚[J].现代预防医学,2018,45(14):2631-2634,2650.
[9] 胡西洲.新型样品前处理技术在环境和生物样品分析中的应用[D].武汉:武汉大学,2012.