制备了聚(丙烯酰胺-乙二醇二甲基丙烯酸酯)(Poly(AA-EGDMA))整体柱,采用红外(IR)光谱、扫描电子显微镜(SEM)对其结构和形貌进行了表征。基于此,建立了Poly(AA-EGDMA)整体柱毛细管微萃取(CME)-等离子体质谱(ICP-MS)联用检测生物样品中痕量重金属离子的分析方法。对影响CME的诸多条件,如样品溶液的pH值、上样体积、上样流速、解吸剂浓度及体积、解吸剂流速以及共存离子的干扰等进行了详细的考察。在优化的实验条件下,方法对Cd2+和Pb2+的检出限分别为4ng·L-1和36ng·L-1,相对标准偏差(c=0.2μg·L-1,n=7)分别为4.7%和3.9%。该整体柱对Cd2+和Pb2+的吸附容量分别为46.7μg·m-1和130μg·m-1。将所建立的方法用于尿样中痕量重金属离子Cd2+、Pb2+的测定,加标回收率分别为99%和100%。
Herein,apoly(acrylamide-co-ethylene glycol dimethacrylate)(Poly(AA-EGDMA))monolithic column was prepared by in situ polymerization and characterized by Fourier infrared spectroscopy(FT-IR)and scanning electron microscope(SEM).Based on it,a method of poly(AA-EGDMA)monolithic column capillary microextraction(CME)-inductively coupled plasma mass spectrometry(ICP-MS)was developed for the determination of trace heavy metal ions in biological samples.Various influencing parameters(such as sample pH,eluent concentration,elution volume,flow rates of eluent and sample solution,sample volume,co-exsiting ions)affecting CME of target analytes were studied in detail.Under the optimal experimental conditions,the detection limits obtained by the proposed method were 4ng·L-1 and36ng·L-1 with the relative standard deviations of 4.7% and 3.9%(c=0.2μg·L-1,n=7)for Cd2+and Pb2+,respectively.The adsorption capacities of poly(AA-EGDMA)monolithic column were 46.7μg·m-1 and130μg·m-1 for Cd2+and Pb2+,respectively.The proposed method was successfully applied to the analysis of trace Pb2+and Cd2+in human urine sample.