分子荧光光谱法在荧光增白剂分析中的应用
发布时间：2019-06-27 14:28
【摘要】：在现代工业生产的各类产品中,荧光增白剂是重要的添加剂。但是在某些涉及人类健康的产品中,荧光增白剂过量使用产生了严重的社会问题。近年来,非法滥用荧光增白剂的现象比较严重,引起了社会的广泛关注。为了消费者的安全与健康,研究和制定行之有效的荧光增白剂定性及定量检测方法迫在眉睫。本论文研究了现代工业生产中常用的四种荧光增白剂(CBS、VBL、CXT、BBU),运用传统分子荧光光谱法、共振光散射光谱法、同步荧光光谱法、纸上荧光-数码比色法和三维荧光光谱法等方法建立了新的检测方法,将这些方法应用于洗衣液、餐巾纸和食用菌中荧光增白剂的定性定量分析,取得了较好的效果。具体的研究内容如下:1、建立了共振光散射光谱法测定荧光增白剂(VBL)的新方法并将其用于测定餐巾纸样品。在λex=λem=469 nm处,共振光散射强度最大,且共振光散射强度与VBL浓度成良好的线性关系,标准曲线为:y=9.70x+17.70,相关系数R=0.9978,线性范围0.01-4.0μg/mL,检出限0.03μg/mL,能达到一般检测的要求。初步探讨了实验用水纯度和pH对VBL溶液的稳定性影响以及样品前处理条件的优化。新的分析方法取得了令人满意的结果。2、建立了共振光散射光谱法定量测定荧光增白剂(CXT)的方法并将其用于食用菌分析。同时对表面活性剂(CTAB)增敏CXT的机理进行了探究。新方法表明,在λex=λem=405 nm处有一个较稳定的共振光散射峰,并且它的强度与CXT的浓度成线性关系,标准曲线为:y=13.45x-1.58,相关系数R=0.9985,线性范围为0.5-15.0μg/mL,检出限为0.09μg/mL。初步探讨了溶液的pH、样品前处理条件的优化以及表面活性剂(CTAB)增敏CXT的条件。结果说明CTAB与CXT之间有稳定缔合物形成,导致荧光增强,使样品测定的灵敏度增加。此分析方法结果令人满意。3、建立了纸上荧光-数码比色法定量测定洗衣液中荧光增白剂(CBS)的新方法。利用微量进样器取样点在定性滤纸上,在黑暗条件下紫外灯下普通数码相机拍摄样点所成的荧光图像进行分析,图像样点灰度面积的积分值与CBS的浓度在一定范围内存在线性关系。在点样体积为2μL条件下,浓度为1.0-40.0μg/mL范围内具有较好的线性关系:y=2031.7x+7196.5,相关系数R=0.9952,将该法用于分析实际样品,无需使用分析仪器,最终结果与荧光分光光度法一致。4、采用多种分子荧光光谱法定性检测了四种荧光增白剂,运用传统荧光光谱法、共振光散射光谱法、同步荧光光谱法以及三维荧光光谱法分别扫描荧光增白剂CBS、VBL、CXT、BBU的水溶液和无水乙醇溶液的荧光光谱。获得的几种荧光光谱对不同的荧光增白剂有很好的区分性。通过荧光激发光谱和发射光谱的组合以及三维荧光光谱,扫描所获得的各荧光增白剂荧光光谱图,各个谱图峰的位置拐点均不一致,可以作为良好的区分各种荧光增白剂的方法。为荧光增白剂的光谱分析积累了基础数据。以上对于荧光增白剂检测方法的研究结果表明,这些方法都具有分析速度快、检测灵敏度高、分析成本低廉等特点。本论文建立的新方法能提供荧光增白剂检测的特征信息,可实现快速鉴定各类产品中的微量痕量的荧光增白剂。
[Abstract]:In the various products of modern industrial production, the fluorescent whitening agent is an important additive. In some products involving human health, however, excessive use of the fluorescent whitening agent produces a serious social problem. In recent years, the phenomenon of the illegal use of the fluorescent whitening agent is more serious, which causes the wide attention of the society. It is urgent to study and develop effective fluorescent whitening agent qualitative and quantitative detection for the safety and health of consumers. The four kinds of fluorescent whitening agents (CBS, VBL, CXT, and BBU), which are commonly used in modern industrial production, are studied in this paper. The new detection method was established by fluorescence-digital colorimetric method and three-dimensional fluorescence spectrometry, and the method was applied to the qualitative and quantitative analysis of the fluorescent whitening agent in the washing liquid, the napkin and the edible fungus, and the better results were obtained. The specific content of the study is as follows:1. The new method for the determination of the fluorescent whitening agent (VBL) by the resonance light scattering spectrometry is established and used to determine the sample of the napkin. The light scattering intensity of the resonance light is the largest at the position of Apex = Ahem = 469nm, and the resonance light scattering intensity is a good linear relationship with the VBL concentration. The standard curve is: y = 9.70x + 17.70, the correlation coefficient R = 0.9978, the linear range of 0.01-4.0 & mu; g/ mL, the detection limit of 0.03 & mu; g/ mL, and the general detection requirement can be met. The effects of water purity and pH on the stability of VBL solution and the optimization of pretreatment conditions were discussed. The new analytical method has obtained satisfactory results.2. The method of quantitative determination of the fluorescent whitening agent (CXT) by the resonance light scattering spectrometry is established and used for the analysis of the edible fungi. The mechanism of the sensitivity of the surfactant (CTAB) to the CXT was also discussed. The new method shows that there is a stable resonance light scattering peak at the position of Apex = Ahem = 405 nm, and its intensity is linear with the concentration of the CXT. The standard curve is: y = 13.45x-1.58, the correlation coefficient R = 0.9985, the linear range is 0.5-15.0. m u.g/ mL, and the detection limit is 0.09. m u.g/ mL. The pH of the solution, the optimization of the pretreatment conditions of the sample and the conditions of the sensitivity of the surfactant (CTAB) to the CXT were discussed. The results show that there is a stable association between CTAB and CXT, which results in the increase of fluorescence and the increase of the sensitivity of the sample. The result of this analytical method is satisfactory.3, a new method for quantitative determination of the fluorescent whitening agent (CBS) in the laundry liquid is established. The fluorescence image of the sampling point of the ordinary digital camera under the dark condition is analyzed by using the sampling point of the micro sample injector on the qualitative filter paper, and the integral value of the gray area of the image sample and the concentration of the CBS have a linear relationship within a certain range. Under the condition of sample volume of 2 & mu; L, the concentration is in the range of 1.0-40.0 & mu; g/ mL and has a good linear relationship: y = 2031.7 x + 7196.5, the correlation coefficient R = 0.9952, the method is used for analyzing the actual sample, no analytical instrument is needed, and the final result is consistent with the fluorescence spectrophotometry. The four fluorescent whitening agents are qualitatively detected by a plurality of molecular fluorescence spectroscopy methods, and the fluorescent whitening agents CBS, VBL and CXT are respectively scanned by using the traditional fluorescence spectroscopy, the resonance light scattering spectroscopy, the synchronous fluorescence spectroscopy and the three-dimensional fluorescence spectroscopy, The aqueous solution of the BBU and the fluorescence spectrum of the absolute ethyl alcohol solution. The obtained fluorescence spectra have good distinguishing properties for different fluorescent whitening agents. By the combination of the fluorescence excitation spectrum and the emission spectrum and the three-dimensional fluorescence spectrum, the fluorescence spectrum of each fluorescent whitening agent obtained by scanning is not consistent with the position inflection point of each spectrum map peak, and the method can be used as a good method for distinguishing various fluorescent whitening agents. And the basic data is accumulated for the spectral analysis of the fluorescent whitening agent. The results show that the method has the characteristics of fast analysis speed, high detection sensitivity, low analysis cost and the like. The new method established in this paper can provide the characteristic information of the detection of the fluorescent whitening agent, and can realize the rapid identification of trace amount of the fluorescent whitening agent in various products.
【学位授予单位】：四川师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.3
本文编号：2506873
[Abstract]:In the various products of modern industrial production, the fluorescent whitening agent is an important additive. In some products involving human health, however, excessive use of the fluorescent whitening agent produces a serious social problem. In recent years, the phenomenon of the illegal use of the fluorescent whitening agent is more serious, which causes the wide attention of the society. It is urgent to study and develop effective fluorescent whitening agent qualitative and quantitative detection for the safety and health of consumers. The four kinds of fluorescent whitening agents (CBS, VBL, CXT, and BBU), which are commonly used in modern industrial production, are studied in this paper. The new detection method was established by fluorescence-digital colorimetric method and three-dimensional fluorescence spectrometry, and the method was applied to the qualitative and quantitative analysis of the fluorescent whitening agent in the washing liquid, the napkin and the edible fungus, and the better results were obtained. The specific content of the study is as follows:1. The new method for the determination of the fluorescent whitening agent (VBL) by the resonance light scattering spectrometry is established and used to determine the sample of the napkin. The light scattering intensity of the resonance light is the largest at the position of Apex = Ahem = 469nm, and the resonance light scattering intensity is a good linear relationship with the VBL concentration. The standard curve is: y = 9.70x + 17.70, the correlation coefficient R = 0.9978, the linear range of 0.01-4.0 & mu; g/ mL, the detection limit of 0.03 & mu; g/ mL, and the general detection requirement can be met. The effects of water purity and pH on the stability of VBL solution and the optimization of pretreatment conditions were discussed. The new analytical method has obtained satisfactory results.2. The method of quantitative determination of the fluorescent whitening agent (CXT) by the resonance light scattering spectrometry is established and used for the analysis of the edible fungi. The mechanism of the sensitivity of the surfactant (CTAB) to the CXT was also discussed. The new method shows that there is a stable resonance light scattering peak at the position of Apex = Ahem = 405 nm, and its intensity is linear with the concentration of the CXT. The standard curve is: y = 13.45x-1.58, the correlation coefficient R = 0.9985, the linear range is 0.5-15.0. m u.g/ mL, and the detection limit is 0.09. m u.g/ mL. The pH of the solution, the optimization of the pretreatment conditions of the sample and the conditions of the sensitivity of the surfactant (CTAB) to the CXT were discussed. The results show that there is a stable association between CTAB and CXT, which results in the increase of fluorescence and the increase of the sensitivity of the sample. The result of this analytical method is satisfactory.3, a new method for quantitative determination of the fluorescent whitening agent (CBS) in the laundry liquid is established. The fluorescence image of the sampling point of the ordinary digital camera under the dark condition is analyzed by using the sampling point of the micro sample injector on the qualitative filter paper, and the integral value of the gray area of the image sample and the concentration of the CBS have a linear relationship within a certain range. Under the condition of sample volume of 2 & mu; L, the concentration is in the range of 1.0-40.0 & mu; g/ mL and has a good linear relationship: y = 2031.7 x + 7196.5, the correlation coefficient R = 0.9952, the method is used for analyzing the actual sample, no analytical instrument is needed, and the final result is consistent with the fluorescence spectrophotometry. The four fluorescent whitening agents are qualitatively detected by a plurality of molecular fluorescence spectroscopy methods, and the fluorescent whitening agents CBS, VBL and CXT are respectively scanned by using the traditional fluorescence spectroscopy, the resonance light scattering spectroscopy, the synchronous fluorescence spectroscopy and the three-dimensional fluorescence spectroscopy, The aqueous solution of the BBU and the fluorescence spectrum of the absolute ethyl alcohol solution. The obtained fluorescence spectra have good distinguishing properties for different fluorescent whitening agents. By the combination of the fluorescence excitation spectrum and the emission spectrum and the three-dimensional fluorescence spectrum, the fluorescence spectrum of each fluorescent whitening agent obtained by scanning is not consistent with the position inflection point of each spectrum map peak, and the method can be used as a good method for distinguishing various fluorescent whitening agents. And the basic data is accumulated for the spectral analysis of the fluorescent whitening agent. The results show that the method has the characteristics of fast analysis speed, high detection sensitivity, low analysis cost and the like. The new method established in this paper can provide the characteristic information of the detection of the fluorescent whitening agent, and can realize the rapid identification of trace amount of the fluorescent whitening agent in various products.
【学位授予单位】：四川师范大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：O657.3
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