聚苯乙烯纳米探针与丁二酮肟反应耦合共振瑞利散射-能量转移光谱法测定痕量尿素

doi:10.3964/j.issn.1000-0593(2020)11-3590-04

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摘要：尿素是氨基酸代谢的最终产物，其作为氮肥在农业中用途广泛。但当尿素的浓度在人体中积累到一定值时，它将对人体的器官将产生一定的损害。因此，建立一种简便、灵敏的尿素检测方法具有重要的意义。共振瑞利散射（RRS）是一种操作简便，灵敏度好及耗能低的分子光谱技术，其在化学及生命科学等领域都得到了广泛的应用。目前，共振瑞利散射技术应用于尿素的定量分析亦有报道，但还是存在操作复杂和灵敏度低等问题。该工作开发了一种简单、快速及灵敏的共振瑞利散射-能量转移（RRS-ET）新方法应用于人体尿液中痕量尿素（UR）的检测。在盐酸及稳定剂氨基硫脲（TSC）存在条件下，丁二酮肟（DMG）与UR反应生成稳定的红色二嗪衍生物4，5-二甲基-2-咪唑酮（DIK），DIK作为能量受体能与能量供体聚苯乙烯纳米探针（PS）发生RRS-ET现象，使得体系的RRS信号发生变化。在一定范围内，随着UR浓度的增大，体系在500 nm处的RRS强度呈线性降低。为了达到最佳检测效果，对影响体系信号的因素进行了优化，结果表明，当选择HCl溶液浓度为0.75 mol·L^-1，TSC溶液浓度为0.22 mmol·L^-1，DMG溶液浓度为19.35 mmol·L^-1，PS的浓度为17.5 μg·mL^-1，水浴温度为80 ℃，水浴反应时间为20 min时，体系获得最佳检测效果。在最佳条件下，聚苯乙烯纳米微粒体系的共振瑞利散射信号降低值与UR浓度在2.0～3200 ng·mL^-1范围内呈线性关系，检出限为2.0 ng·mL^-1。同时，考察了共存物质对2 000 ng·mL^-1 UR测定情况的影响。结果表明，100 μg·mL^-1的Na⁺，Zn²⁺，20 μg·mL^-1的Mn²⁺，Cr³⁺，10 μg·mL^-1的SO^2-₄，NO^-₃，Co²⁺，Fe³⁺，2 μg·mL^-1 Cr⁶⁺，Ca²⁺不干扰UR的测定，说明该方法有较好的选择性。最后，将该RRS-ET方法应用于尿液中UR的测定，样品加标回收率在94.19%～96.94%之间，相对标准偏差（RSD）在4.20%～6.35%之间，检测结果令人满意。据此，建立了一个共振瑞利散射-能量转移分析尿素的新方法，方法操作简单、灵敏度高。

关键词：聚苯乙烯纳米微粒；尿素；丁二酮肟；共振瑞利散射；能量转移

Abstract：Urea is the final product of amino acid metabolism and is widely used in agriculture as a nitrogen fertilizer. However, when the concentration of urea accumulates to a certain value in the human body, it will cause certain damage to the organs of the human body. Therefore, it is of great significance to establish a simple and sensitive method for urea detection. Resonance Rayleigh Scattering (RRS) is a molecular spectroscopy technique with simple operation, good sensitivity and low energy consumption. It has been widely used in the fields of chemistry and life sciences. At present, the application of the resonance Rayleigh scattering technique to the quantitative analysis of urea has also been reported, but there are still problems such as complicated operation and low sensitivity. In this paper, a simple, rapid and sensitive resonant Rayleigh scattering-energy transfer (RRS-ET) method is developed for the detection of trace urea (UR) in human urine. In the presence of HCl and the stabilizer thiosemicarbazone (TSC), dimethylglyoxime (DMG) can react with UR to form a stable red diazine derivative of 4,5-dimethyl-2-imidazolidone (DIK). The RRS-ET phenomenon occurs between DIK as an energy acceptor and an energy donor polystyrene nanoprobe (PS), which causes the RRS signal of the system to change. Within a certain range, as the UR concentration increases, the RRS intensity at 500 nm decreases linearly. In order to achieve the best detection results, the factors affecting the system signal are optimized. The results show that when the concentration of HCl solution is 0.75 mol·L^-1, the concentration of TSC solution is 0.22 mmol·L^-1, the concentration of DMG solution is 19.35 mmol·L^-1, the concentration of PS is 17.5 μg·mL^-1, the temperature of the water bath is 80 ℃, and the bath time is 20 min, the system obtains the best detection effect. Under the optimal conditions, the resonance Rayleigh scattering signal reduction value of the polystyrene nanoparticle system is linear with the UR concentration in the range of 2.0～3 200 ng·mL^-1, and the detection limit is 2.0 ng·mL^-1. At the same time, the effect of coexisting substances on the determination of 2 000 ng·mL^-1 UR is investigated. The results show that 100 μg·mL^-1 of Na⁺, Zn²⁺, 20 μg·mL^-1 of Mn²⁺, Cr³⁺, 10 μg·mL^-1 of SO^2-₄, NO^-₃, Co²⁺, Fe³⁺, 2 μg·mL^-1 Cr⁶⁺ and Ca²⁺ did not interfere with UR determination. The results show that the method has good selectivity. Finally, the RRS-ET method is applied to the determination of UR in the urine. The recovery of the spiked samples is 94.19%～96.94%, and the relative standard deviation (RSD) is 4.20%～6.35%. The test results are satisfactory. Based on this, a new method of resonance Rayleigh scattering-energy transfer analysis of urea is established with simple operation and high sensitivity.

Key words：Polystyrene nanoparticles; Urea; Dimethylglyoxime; Resonance Rayleigh scattering; Energy transfer

收稿日期: 2019-11-22 修订日期: 2020-03-06

中图分类号:

O657.39

基金资助: 国家自然科学基金项目(21767004, 21667006)及珍稀濒危动植物生态与环境保护教育部重点实验室研究基金项目（ERESP2018201）资助

通讯作者: 蒋治良 E-mail: zljiang@mailbox.gxnu.edu.cn

作者简介: 姚东梅，1985年生，广西师范大学化学与药学学院博士研究生 e-mail: dmyao47@163.com

引用本文:

姚东梅，卢珊珊，温桂清，梁爱惠，蒋治良. 聚苯乙烯纳米探针与丁二酮肟反应耦合共振瑞利散射-能量转移光谱法测定痕量尿素[J]. 光谱学与光谱分析, 2020, 40(11): 3590-3593.
YAO Dong-mei, LU Shan-shan, WEN Gui-qing, LIANG Ai-hui, JIANG Zhi-liang. Determination of Trace Urea by Resonance Rayleigh Scattering-Energy Transfer Spectroscopy Coupled With Polystyrene Nanoprobe and Dimethylglyoxime Reaction. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2020, 40(11): 3590-3593.

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