磁性氧化石墨烯固相萃取-液质联用检测尿液中核苷

Determination of Nucleosides in Urine by Magnetic Graphene Oxide Solid Phase Extraction Coupled with Liquid Mass Spectrometry

以磁性氧化石墨烯(Fe_(3)O_(4)@GO)纳米材料为磁性固相萃取吸附剂,建立固相萃取-液质联用法分析尿液中的尿苷、肌苷、胞苷、腺苷。制备Fe_(3)O_(4)@GO纳米材料,用透射电镜、红外光谱、X射线衍射对其进行结构表征。以Fe_(3)O_(4)@GO纳米复合材料用作吸附剂,对尿液中的核苷进行前处理。考察最佳萃取条件,包括pH值、吸附剂用量、吸附时间等。磁性固相萃取后,用液质联用进行检测,线性范围为5~200 ng/mL时,该方法线性关系良好(R^(2)>0.999),添加水平在100 ng/L时,加标回收率为60.1%~105.6%,相对标准偏差在1.17%~3.56%,具有操作简便、稳定高效等特点,为尿液中核苷含量定量分析提供了一种简单可靠的方法。

Using Fe_(3)O_(4)@GO nanomaterial as magnetic SPE adsorbent,a SPE-MS method was established for the determination of uridine,inosine,cytosine and adenosine in urine.The magnetic Fe_(3)O_(4)@GO nanomaterials were prepared and characterized by transmission electron microscopy,infrared spectroscopy and X-ray diffraction.The nucleosides in urine were pretreated with Fe_(3)O_(4)@GO nanocomposite as adsorbent.The optimum extraction conditions,including pH,adsorbent dosage and adsorption time,were investigated.After magnetic solid phase extraction,the method was detected by liquid mass spectrometry.The linear range was 5~200 ng/mL,and the method had a good linear relationship(R^(2)>0.999).When the supplemental level was 100 ng/L,the recoveries were 60.1%~105.6%,and the relative standard deviations were 1.17%~3.56%.It has the characteristics of simple operation,stability and high efficiency,and provides a simple and reliable method for quantitative analysis of nucleoside content in urine.