柱前衍生-高效液相色谱法测定人尿中硫氰酸盐
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摘要
目的建立以五氟苄基溴作为柱前衍生试剂,高效液相色谱法测定人尿中硫氰酸盐的方法。方法尿样中硫氰酸盐与五氟苄基溴衍生后,经多孔层120EC-C18色谱柱分离,以乙腈:去离子水(60:40,V/V)为流动相,经高效液相色谱-紫外检测器检测,检测波长为212 nm。结果尿中硫氰酸盐质量浓度为0.05~10.32 mg/L时线性关系良好,线性相关系数为0.999;检出限为6.31μg/L,最低检出浓度为63.10μg/L(以尿样体积0.1 mL计);加标回收率为95.1%~102.9%;批内相对标准偏差(RSD)为0.9%~1.0%,批间RSD为0.9%~2.1%;在4℃样品可保存7 d。结论本法灵敏度高、特异性好、样品前处理简单,可用于职业人群尿中硫氰酸盐的测定。
Objective To establish a method for detecting thiocyanate in human urine by high performance liquid chromatography( HPLC) with 2,3,4,5,6-pentafluorobenzyl bromide as precolumn derivatization reagent.Methods Thiocyanate in human urine was derived with 2,3,4,5,6-pentafluorobenzyl bromide, and separated by poroshell 120EC-C18 column with acetonitrile:deionized water( 60:40,V/V) as mobile phase.detected by HPLC,Liquid chromatography-UV detector was used for determination.The wavelength was 212.00 nm.Results Good linearity was obtained in the range of 0.05-10.32 mg/L with the correlation coefficient of 0.999.The detection limit was 6.31 μg/L and the minimum detection concentration was 63.10 μg/L( 0.1 mL urine).The recovery rate was 95.1%-102.9%.The within-run relative standard deviation( RSD) and the between-run RSD were 0.9%-1.0% and 0.9%-2.1%,respectively.The urine samples could be stored at 4 ℃ for 7 days.Conclusion This method has high sensitivity,good specificity and sample preparation,which can be used for detecting urine thiocyanate in occupational population.
Objective To establish a method for detecting thiocyanate in human urine by high performance liquid chromatography( HPLC) with 2,3,4,5,6-pentafluorobenzyl bromide as precolumn derivatization reagent.Methods Thiocyanate in human urine was derived with 2,3,4,5,6-pentafluorobenzyl bromide, and separated by poroshell 120EC-C18 column with acetonitrile:deionized water( 60:40,V/V) as mobile phase.detected by HPLC,Liquid chromatography-UV detector was used for determination.The wavelength was 212.00 nm.Results Good linearity was obtained in the range of 0.05-10.32 mg/L with the correlation coefficient of 0.999.The detection limit was 6.31 μg/L and the minimum detection concentration was 63.10 μg/L( 0.1 mL urine).The recovery rate was 95.1%-102.9%.The within-run relative standard deviation( RSD) and the between-run RSD were 0.9%-1.0% and 0.9%-2.1%,respectively.The urine samples could be stored at 4 ℃ for 7 days.Conclusion This method has high sensitivity,good specificity and sample preparation,which can be used for detecting urine thiocyanate in occupational population.
引文
[1]龚敏莉,李波,郝玲妹.丙烯腈从业人员及宁波市居民尿硫氰酸盐水平调查[J].中国卫生检验杂志,2016,26(7):1038-1039.
[2]闫若玉,龚辉,吴炜,等.低浓度丙烯腈暴露作业人员健康监护指标分析[J].职业卫生与应急救援,2011,29(2):76-80.
[3]李环,郑扬,艾丽莎.丙烯腈作业工人尿硫氰酸盐水平及健康效应[J].环境与职业医学,2012,29(9):561-562.
[4]王升.尿中硫氰酸根(SCN-)测定方法的研究[D].北京:中国疾病控制中心职业卫生所,2017.
[5]周元陵.尿硫氰酸盐在丙烯腈职业健康监护中的作用[D].上海:复旦大学,2002.
[6]钱小莲,宋海燕,柏建岭.某食品企业149名健康工人尿中硫氰酸盐水平分析[J].中华劳动卫生职业病杂志,2012,30(8):595-596.
[7]宋振威,郭平,刘文卫.无锡地区健康人群尿硫氰酸盐正常参考值调查[J].职业卫生与应急救援,2017,35(1):46-47.
[8]冯翠霞,林丽玲,黄辉涛.分光光度法测定尿中硫氰酸盐的异烟酸-吡唑酮[J].中国职业医学,2009,36(6):501-501.
[9]SONG J,WU F Y,WAN Y Q,et al.Ultrasensitive turn-on fluorescent detection of trace thiocyanate based on fluorescence resonance energy transfer[J].Talanta,2015,132:619-624.
[10]李滢倩.离子色谱和高效液相色谱测定牛乳中硫氰酸盐含量的研究[D].长春:吉林大学,2010.
[11]MA Y J,LI M,YU H,et al.Fast analysis of thiocyanate by ion-pair chromatography with direct conductivity detection on a monolithic column[J].Chinese Chem Lett,2013,24(12):1067-1069.
[12]中华人民共和国卫生部.尿中硫氰酸盐的吡啶-巴比妥酸分光光度法:WS/T 39—1996[S].北京:人民卫生出版社,1997.
[13]蔡秀丽,施逸岚,陈建忠.人尿中硫氰酸盐的快速测定方法[J].中国卫生检验杂志,2015(11):1703-1704.
[14]符展明,吴梦奎.顶空气相色谱法测定水中微量硫氰酸根[J].环境与健康杂志,1991,8(6):270-272.
[15]韩菊,高文惠.衍生气相色谱法测定人尿中硫氰酸根[J].环境与健康杂志,1999,16(3):175-175.
[16]刘晓宇,云自厚.化学衍生-高效液相色谱法测定硫氰酸根阴离子[J].分析化学,1993,21(10):1199-1201.
[17]刘晓宇,云自厚.衍生气相色谱法测定人尿和唾液中微量硫氰酸根[J].环境与健康杂志,1994,11(3):130-131.
[18]中华人民共和国卫生部.职业卫生标准制定指南第5部分:生物材料中化学物质测定方法:GBZ/T 210.5—2008[S].北京:人民卫生出版社,2008.
[2]闫若玉,龚辉,吴炜,等.低浓度丙烯腈暴露作业人员健康监护指标分析[J].职业卫生与应急救援,2011,29(2):76-80.
[3]李环,郑扬,艾丽莎.丙烯腈作业工人尿硫氰酸盐水平及健康效应[J].环境与职业医学,2012,29(9):561-562.
[4]王升.尿中硫氰酸根(SCN-)测定方法的研究[D].北京:中国疾病控制中心职业卫生所,2017.
[5]周元陵.尿硫氰酸盐在丙烯腈职业健康监护中的作用[D].上海:复旦大学,2002.
[6]钱小莲,宋海燕,柏建岭.某食品企业149名健康工人尿中硫氰酸盐水平分析[J].中华劳动卫生职业病杂志,2012,30(8):595-596.
[7]宋振威,郭平,刘文卫.无锡地区健康人群尿硫氰酸盐正常参考值调查[J].职业卫生与应急救援,2017,35(1):46-47.
[8]冯翠霞,林丽玲,黄辉涛.分光光度法测定尿中硫氰酸盐的异烟酸-吡唑酮[J].中国职业医学,2009,36(6):501-501.
[9]SONG J,WU F Y,WAN Y Q,et al.Ultrasensitive turn-on fluorescent detection of trace thiocyanate based on fluorescence resonance energy transfer[J].Talanta,2015,132:619-624.
[10]李滢倩.离子色谱和高效液相色谱测定牛乳中硫氰酸盐含量的研究[D].长春:吉林大学,2010.
[11]MA Y J,LI M,YU H,et al.Fast analysis of thiocyanate by ion-pair chromatography with direct conductivity detection on a monolithic column[J].Chinese Chem Lett,2013,24(12):1067-1069.
[12]中华人民共和国卫生部.尿中硫氰酸盐的吡啶-巴比妥酸分光光度法:WS/T 39—1996[S].北京:人民卫生出版社,1997.
[13]蔡秀丽,施逸岚,陈建忠.人尿中硫氰酸盐的快速测定方法[J].中国卫生检验杂志,2015(11):1703-1704.
[14]符展明,吴梦奎.顶空气相色谱法测定水中微量硫氰酸根[J].环境与健康杂志,1991,8(6):270-272.
[15]韩菊,高文惠.衍生气相色谱法测定人尿中硫氰酸根[J].环境与健康杂志,1999,16(3):175-175.
[16]刘晓宇,云自厚.化学衍生-高效液相色谱法测定硫氰酸根阴离子[J].分析化学,1993,21(10):1199-1201.
[17]刘晓宇,云自厚.衍生气相色谱法测定人尿和唾液中微量硫氰酸根[J].环境与健康杂志,1994,11(3):130-131.
[18]中华人民共和国卫生部.职业卫生标准制定指南第5部分:生物材料中化学物质测定方法:GBZ/T 210.5—2008[S].北京:人民卫生出版社,2008.