磁性纳米材料固相微萃取-高效液相色谱法测定尿中苯巯基尿酸

Determination of S-phenylmercapturic acid in urine by solid phase microextraction coupled with high performance liquid chromatography

目的建立葡萄糖包裹的Fe_3O_4磁性纳米材料分散固相微萃取结合高效液相色谱测定尿液中苯巯基尿酸的方法。方法本实验先采用化学共沉淀法制备Fe_3O_4磁核,再用水热法合成葡萄糖包裹Fe_3O_4磁核的复合材料。对制得Fe_3O_4@GLU磁性纳米材料利用红外光谱技术进行表征。对SPMA的分散固相微萃取条件进行了优化,分别考察了吸附时间、吸附剂用量、样品溶液p H值、洗脱剂和洗脱时间。取5 ml尿样,用盐酸调节pH值<2.0,利用磁性纳米材料进行分散固相微萃取,经C18柱(C18柱:250 mm×4.6 mm,4μm)分离,采用紫外检测器检测,以保留时间定性,峰面积定量。结果本法在0.050 mg/L^1.0 mg/L浓度范围内呈线性,相关系数为0.999 7,方法检出限为0.003 mg/L。样品加标回收率为96.1%~104.7%;批内精密度为2.36%~3.95%(n=6),批间精密度为7.60%~8.42%(n=6)。结论本法简单实用,有机试剂用量少,灵敏度高,可以满足尿样中苯巯基尿酸检测的要求。

Objective A method for the determination of S-phenylmercapturic acid（ S-PMA） in urine by dispersive solid-phase extraction and high performance liquid chromatography（ HPLC） with glucose bonded Fe3 O4 magnetic nanocomposite（ Fe3 O4@ GLU） was successfully developed. Methods In this experiment,the Fe3 O4 magnetic core was prepared by chemical co-precipitation method,and the composite material of glucose-coated Fe3 O4 magnetic core was synthesized by hydrothermal method. The prepared Fe3 O4@ GLU was characterized by infrared spectrometer（ IR）. The dispersed solid phase microextraction conditions of SPMA were optimized,and the adsorption time,the amount of adsorbent,the p H of sample solution,the eluent amount and the elution time were investigated. The 5 ml urine samples were adjusted to p H 2. 0 and extracted by Fe3 O4@ GLU. The magnetic nanomaterials were used for dispersion solid phase microextraction, separated by C18 column（ C18 column： 250 mm × 4. 6 mm,4 μm）,detected by UV detector,and characterized by retention time and peak area.Results The method showed good linearity in the range of 0. 050 mg/L-1. 0 mg/L,and the relative coefficient（ r） was 0. 999 7.The detect limit of SPMA was 0. 003 g/L. The spiked recovery ranged from 96. 1% to 104. 7%. The intra-day and inter-day precisions（ RSD） were within 2. 36%-3. 95% and 7. 60%-8. 42%,respectively. Conclusion The method is simple,practical and high sensitive,which needs little organic reagent and can meet the requirements of S-phenylmercapturic acid detection in urine samples.