摘要
目的建立硅藻土改性磁性纳米材料分散固相萃取-高效液相色谱测定尿中苯巯基尿酸。方法尿样经过离心后,取5. 0 ml上清液,用盐酸调节pH值为1. 0,经硅藻土改性磁性纳米材料进行分散固相萃取后,分离出有机相,残渣用甲醇溶解并定容后注入高效液相色谱仪,经EC-C18反相色谱柱(150 mm×4. 6 mm,4μm)分离,紫外检测器检测,以保留时间定性,峰面积外标法定量。结果本法中苯巯基尿酸在0. 050 mg/L～1. 0 mg/L内线性关系良好,相关系数为0. 999 7,以3倍噪音值计算方法检出限为0. 028 mg/L,在0. 050 mg/L～1. 0 mg/L内添加低、中、高3个浓度水平,样品加标回收率为94. 9%～108. 0%,批内精密度和批间精密度分别为4. 6%～9. 8%(n=6)与4. 3%～8. 9%(n=6)。结论本方法简便快捷,分析时间短,灵敏度高,可用于职业接触苯人群尿中苯巯基尿酸的检测。
Objective A method based on diatomite bonded Fe_3 O4 magnetic nanocomposite（DBMNPs） as adsorbent was developed for the determination of S-phenylmercapturic acid（SPMA） in urine by dispersive solid-phase extraction and HPLC.Methods The urine sample was centrifugated,and the supernatant of urine samples（5. 0 ml） were collected for pH adjusting to 1. 0 by adding Hcl and extracted with DBMNPs. The extract was re-dissolved in methanol and then the analyte was separated on an EC-C18 column（150 mm × 4. 6 mm,4 μm） and detected by VWD. The S-phenylmercapturic acid was qualified by the retention time and quantified by standard curve method. Results The method showed good linearity in the range of0. 050 mg/L-1. 0 mg/L（r = 0. 999 7）. The detect limit of the method was 0. 028 mg/L（S/N = 3）. The average recovery ranged from 94. 9% to 108. 0% at three spiked levels in the range of 0. 050 mg/L-1. 0 mg/L. The intra-day and inter-day precisions（RSDs） were within 4. 6%-9. 8%（n = 6） and 4. 3%-8. 9%（n = 6）,respectively. Conclusion This method is simple,practical and high sensitive. It can be used to detect SPMA in urine for occupational population exposure to benzene.
作者
单晓月
施燕鹏
谈思维
邵吉
曹承建
叶海朋
SHAN Xiao-yue;SHI Yan-peng;TAN Si-wei;SHAO Ji;CAO Cheng-jian;YE Hai-peng(Hangzhou Occupational Disease Prevention and Control Hospital,Hangzhou,Zhejiang 310014,China)
出处
《中国卫生检验杂志》
CAS
2018年第19期2309-2312,共4页
Chinese Journal of Health Laboratory Technology
基金
浙江省医药卫生科技计划项目(2016KYB241
2018KY-640)
杭州市卫生科技计划重点项目(2015Z10)
关键词
苯巯基尿酸
磁性分散固相萃取
高效液相色谱
S - phenylmercapturic acid
Magentic dispersive solid - phase extraction
High performance liquid chromatography
