分子熒光光譜法在熒光增白劑分析中的應(yīng)用
發(fā)布時間：2019-06-27 14:28
【摘要】：在現(xiàn)代工業(yè)生產(chǎn)的各類產(chǎn)品中,熒光增白劑是重要的添加劑。但是在某些涉及人類健康的產(chǎn)品中,熒光增白劑過量使用產(chǎn)生了嚴(yán)重的社會問題。近年來,非法濫用熒光增白劑的現(xiàn)象比較嚴(yán)重,引起了社會的廣泛關(guān)注。為了消費者的安全與健康,研究和制定行之有效的熒光增白劑定性及定量檢測方法迫在眉睫。本論文研究了現(xiàn)代工業(yè)生產(chǎn)中常用的四種熒光增白劑(CBS、VBL、CXT、BBU),運用傳統(tǒng)分子熒光光譜法、共振光散射光譜法、同步熒光光譜法、紙上熒光-數(shù)碼比色法和三維熒光光譜法等方法建立了新的檢測方法,將這些方法應(yīng)用于洗衣液、餐巾紙和食用菌中熒光增白劑的定性定量分析,取得了較好的效果。具體的研究內(nèi)容如下:1、建立了共振光散射光譜法測定熒光增白劑(VBL)的新方法并將其用于測定餐巾紙樣品。在λex=λem=469 nm處,共振光散射強度最大,且共振光散射強度與VBL濃度成良好的線性關(guān)系,標(biāo)準(zhǔn)曲線為:y=9.70x+17.70,相關(guān)系數(shù)R=0.9978,線性范圍0.01-4.0μg/mL,檢出限0.03μg/mL,能達到一般檢測的要求。初步探討了實驗用水純度和pH對VBL溶液的穩(wěn)定性影響以及樣品前處理條件的優(yōu)化。新的分析方法取得了令人滿意的結(jié)果。2、建立了共振光散射光譜法定量測定熒光增白劑(CXT)的方法并將其用于食用菌分析。同時對表面活性劑(CTAB)增敏CXT的機理進行了探究。新方法表明,在λex=λem=405 nm處有一個較穩(wěn)定的共振光散射峰,并且它的強度與CXT的濃度成線性關(guān)系,標(biāo)準(zhǔn)曲線為:y=13.45x-1.58,相關(guān)系數(shù)R=0.9985,線性范圍為0.5-15.0μg/mL,檢出限為0.09μg/mL。初步探討了溶液的pH、樣品前處理條件的優(yōu)化以及表面活性劑(CTAB)增敏CXT的條件。結(jié)果說明CTAB與CXT之間有穩(wěn)定締合物形成,導(dǎo)致熒光增強,使樣品測定的靈敏度增加。此分析方法結(jié)果令人滿意。3、建立了紙上熒光-數(shù)碼比色法定量測定洗衣液中熒光增白劑(CBS)的新方法。利用微量進樣器取樣點在定性濾紙上,在黑暗條件下紫外燈下普通數(shù)碼相機拍攝樣點所成的熒光圖像進行分析,圖像樣點灰度面積的積分值與CBS的濃度在一定范圍內(nèi)存在線性關(guān)系。在點樣體積為2μL條件下,濃度為1.0-40.0μg/mL范圍內(nèi)具有較好的線性關(guān)系:y=2031.7x+7196.5,相關(guān)系數(shù)R=0.9952,將該法用于分析實際樣品,無需使用分析儀器,最終結(jié)果與熒光分光光度法一致。4、采用多種分子熒光光譜法定性檢測了四種熒光增白劑,運用傳統(tǒng)熒光光譜法、共振光散射光譜法、同步熒光光譜法以及三維熒光光譜法分別掃描熒光增白劑CBS、VBL、CXT、BBU的水溶液和無水乙醇溶液的熒光光譜。獲得的幾種熒光光譜對不同的熒光增白劑有很好的區(qū)分性。通過熒光激發(fā)光譜和發(fā)射光譜的組合以及三維熒光光譜,掃描所獲得的各熒光增白劑熒光光譜圖,各個譜圖峰的位置拐點均不一致,可以作為良好的區(qū)分各種熒光增白劑的方法。為熒光增白劑的光譜分析積累了基礎(chǔ)數(shù)據(jù)。以上對于熒光增白劑檢測方法的研究結(jié)果表明,這些方法都具有分析速度快、檢測靈敏度高、分析成本低廉等特點。本論文建立的新方法能提供熒光增白劑檢測的特征信息,可實現(xiàn)快速鑒定各類產(chǎn)品中的微量痕量的熒光增白劑。
[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.
【學(xué)位授予單位】：四川師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O657.3
本文編號：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.
【學(xué)位授予單位】：四川師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O657.3
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