摘要
目的建立柱前衍生-气相色谱法测定尿中丁酮的方法。方法尿中丁酮在酸性条件下,加入碘化钾与重铬酸钾,50℃水浴60 min,用正己烷萃取,加入硫代硫酸钠溶液除去多余的碘,离心半径81 mm,10000 r/min离心5 min,吸取上清液,Agilent HP-5色谱柱(30 m×0.32 mm,0.25μm)分析,程序升温,电子捕获检测器(ECD)检测,检测器温度为300℃,进样口温度为200℃,分流比10∶1,氮气为载气。结果丁酮在0.5~10.0 mg/L范围内峰面积与质量浓度线性关系良好,线性相关系数(R)为0.9991~0.9992。低、中、高3个浓度水平的平均加标回收率为97.8%~104.2%,相对标准偏差为1.94%~6.48%(n=6),方法检出限(LOD)与定量限(LOQ)分别为0.06 mg/L(S/N=3)和0.19 mg/L(S/N=10)。结论本法操作简单,灵敏度高,可应用于职业接触人群尿中丁酮测定。
Objective To establish a method for determination of the butanone in urine by gas chromatography(GC)with pre-column derivation.Methods For detecting of butanone in urine,potassium iodide and potassium dichromate were added into urine under acidic condition,sample derivatization was undertaken in 50℃water bath for 60 min and the iodine butanone was extracted with n-hexane.After the sodium thiosulfate solution was used to remove excess iodine,urine samples were centrifuged at 10000 r/min for 5 min,then the supernatant was analyzed using temperature rising programming with the Agilent Hp-5 column(30 m×0.32 mm,0.25μm)and electron capture detector(ECD)as the detector.The detector temperature was 300℃,the inlet temperature was 200℃,and the carrier gas was nitrogen.Results For detecting of butanone in urine,potassium iodide and potassium dichromate were added for derivatization under the acidic condition.After extraction and centrifugation,the supernatant directly put through column and detected by ECD.In present study,the sample pretreatment condition was optimized,the relative standard deviations of intra-day and inner-day,the spiked samples and its recovery were evaluated for analyzing the accuracy of the proposed method.Conclusion This method has proved to be simple,efficient and highly sensitivity,it can be utilized for butanone detection in occupational population.
作者
邵吉
施燕鹏
谈思维
单晓月
苏克文
张玲
叶海朋
Shao Ji;Shi Yanpeng;Tan Siwei;Shan Xiaoyue;Su Kewen;Zhang Ling;Ye Haipeng(Hangzhou Occupational Disease Prevention and Control Hospital,Hangzhou 310014,China)
出处
《中华劳动卫生职业病杂志》
CAS
CSCD
北大核心
2020年第12期940-943,共4页
Chinese Journal of Industrial Hygiene and Occupational Diseases
基金
杭州市医药卫生科技计划项目(0020190983)。
关键词
色谱
气相
丁酮
柱前衍生
尿
电子捕获检测器
Chromatography,Gas(GC)
Butanone
Pre-column derivation
Urine
Electron capture detection(ECD)
