摘要
目的 建立氰化物职业接触人群尿中硫氰酸根(SCN-)的离子色谱测定方法.方法 用50 ml离心管采集作业工人班后尿约20 ml.将稀释后的尿液样品经C18柱预处理,由AS16色谱柱分离,KOH流动相洗脱,电导检测器检测,标准曲线法定量.结果 该方法检测SCN-的线性范围为0.1~5.0μg/ml,r=0.999,方法检出限为0.11 μg/ml,定量下限为0.35 μg/ml,加标回收率为95.1%~99.7%,批内精密度为0.54%~2.05%,批间精密度为2.06%~5.09%.样品置于室温、4℃和-20℃条件下可分别保存5、7和14 d.结论 该方法的各项技术指标均符合GBZ/T 210.5-2008《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》的要求,适用于职业接触氰化物人群尿中代谢产物SCN-浓度的测定.
Objective To establish ion chromatography method to determine thiocyanate within urine of workers who were exposed to cyanide.Methods Mter the workers work,used 50 ml centrifuge tube to collect the urine of workers about 20 ml.The urine were tested by centrifugation,dilution and filtration by C18 column,thiocyanate was separated by AS16 and mobile phase elution by KOH,detected by electrical circuitryconductivity detector,quantitative by the standard curve method.Results The linear correlation coefficient of thiocyanate within the range of 0.1-5.0 μg/ml was more than 0.999.The method detection limit was 0.11 μg/ml (in 1 ml urine),the method quantitative limit was 0.35 μg/ml.The method recoveries were 95.1%-99.7%.The within-day precision range was 0.54%-2.05%,The between-run precision range was 2.06%-5.09%.Sample stability test showed that thiocyanate samples could be stored for 5 days at room temperature and 7 days at 4 ℃,could be stored for 14 days at-20 ℃.Conclusion The technical indicator of method compliance with rule of Guide for establishing occupation health standards-Part 5:determination methods of chemicals in biological materials (GBZ/T 210.5-2008),the method applies to workers who were exposed to cyanide.
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
2017年第3期220-223,共4页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
基金项目:国家科技支撑计划项目(2014BA112800)
卫生部行业公益项目(201402021)
关键词
色谱法
硫氰酸根
离子
尿
Chromatography
Thiocyanate
Ions
Urine