尿镍测定的超声辅助离子液体微萃取-石墨炉原子吸收光谱法  

Determination of nickel in urine by ultrasonic-assisted ionic liquid microextraction-graphite furnace atomic absorption spectrometry

作　　者：任雨萌 梅勇 方若丹 Ren Yumeng;Mei Yong;Fang Ruodan(Hubei Province Key Laboratory of Occupational Hazard Identification and Control,School of Public Health,Wuhan University of Science and Technology,Wuhan 430065,China)

机构地区：[1]武汉科技大学医学院公共卫生学院,武汉科技大学职业危害识别与控制湖北省重点实验室,430065

出　　处：《中华劳动卫生职业病杂志》2020年第10期767-769,共3页Chinese Journal of Industrial Hygiene and Occupational Diseases

摘　　要：目的建立超声辅助离子液体微萃取-石墨炉原子吸收光谱法测定尿中镍的含量。方法于2018年9月至2019年9月,以甲醇为分散剂,吡咯烷二硫代甲酸铵盐为螯合剂,离子液体1-己基-3-甲基-咪唑六氟磷酸盐([Hmim][PF6])为萃取剂,萃取尿中镍;加入pH 9缓冲溶液,超声10 min后,离心弃上清,加无水甲醇溶解沉淀,在涡旋混合仪上充分混匀,取15μl混合液用石墨炉原子吸收光谱法测定。结果尿镍浓度为2.0~10.0μg/L线性关系良好,r=0.999,检出限为0.43μg/L。加标回收率为95.6%~103.7%,相对标准偏差为2.53%~4.82%。结论超声辅助离子液体微萃取-石墨炉原子吸收光谱法测定尿镍的检出限低、回收率高、精密度好,可用于镍职业接触人群和非职业接触人群的尿镍测定。Objective To set up a new method to determine the nickel of urine in urine using dispersive liquid-liquid microextraction(DLLME)coupled with graphite furnace atomic absorption spectrometry(GFAAS).Methods From September 2018 to September 2019,the methanol,pyrrolidine dithiocarbamate and ionic liquid 1-hexyl-3-methyl-imidazolium hexafluorophosphate were used as dispersive solvent,the chelating agent and extraction solvent for the preconcentration of nickel,respectively.After adding into buffer solution of pH 9,ultrasonic dissolving for 10 minutes,centrifugal separation and then discarding the supernatant,the precipitate was saved.Dissolving the precipitate by methanol,mixing thoroughly on a vortex mixer,the 15μl of the mixed solution was used for determination by graphite furnace atomic absorption spectrometry.Results The linear correlation coefficient of urine nickel concentration in the range of 2.0-10.0μg/L,r=0.999,with the detection limitation of 0.43μg/L.The recovery rate and the relative standard deviations were 95.6%-103.7% and 2.53%-4.82%,respectively.Conclusion The method,which has low detection limit,high recovery rate and good precision,is suitable for the determination of nickel in urine for the occupational populations exposure to nickel and non-occupational exposure.

关 键 词：镍 尿 离子液体 超声辅助 石墨炉原子吸收 

分 类 号：R446.1[医药卫生—诊断学]