熒光光譜與共振瑞利散射技術(shù)測定柔紅霉素、美洛昔康和鎘離子的新方法研究
發(fā)布時(shí)間：2018-08-01 14:27
【摘要】：本文主要應(yīng)用熒光光譜與共振瑞利散射技術(shù)對(duì)柔紅霉素、美洛昔康和鎘離子進(jìn)行測定。研究了它們與探針meso-四(4-磺基苯基)卟啉、乙酸雙氧鈾、鄰菲羅啉和赤蘚紅之間的相互作用。文中還結(jié)合吸收光譜和量子化學(xué)計(jì)算來討論其相互作用的機(jī)理,以此建立了測定柔紅霉素、美洛昔康和鎘離子的新方法,并將實(shí)驗(yàn)方法應(yīng)用于實(shí)際樣品的檢測。主要研究內(nèi)容如下： 1.以meso-四(4-磺基苯基)卟啉為探針熒光猝滅法和分光光度法測定柔紅霉素 以合成的meso-四(4-磺基苯基)卟啉(TPPS4)為探針,提出了熒光和吸收光譜測定鹽酸柔紅霉素(DNR)的新方法。在pH4.6的鄰苯二甲酸氫鉀-NaOH緩沖溶液中,TPPS4與DNR通過靜電引力和疏水作用力相互作用,形成1：1的結(jié)合產(chǎn)物,導(dǎo)致TPPS4的熒光猝滅和吸收光譜改變。在最大激發(fā)波長(λex)和最大發(fā)射波長(λem)(λex/λem=435nm/672nm)處檢測體系的熒光強(qiáng)度,實(shí)驗(yàn)發(fā)現(xiàn)TPPS4的熒光猝滅值(AF)與DNR濃度在0.8～6.0mg·L-1呈良好的線性關(guān)系,檢出限為27.0ng·mL-1。同時(shí),體系的吸光度在433nm處逐漸減弱,而在420nm處出現(xiàn)新吸收峰,兩處吸光度變化值(AA)均與DNR濃度在一定范圍遵從比耳定律,摩爾吸光系數(shù)(ε)分別為ε433=7.75x104L·mol-1·cm-1(褪色法),ε420=5.19×104L·mol-1·cm-1(增色法),當(dāng)采用雙波長疊加法時(shí),摩爾吸光系數(shù)可達(dá)1.29×105L·mol-1·cm-1。實(shí)驗(yàn)研究了熒光猝滅反應(yīng)的適宜條件和影響因素,考察了共存物質(zhì)的影響,表明方法具有較好的選擇性,適用于血樣和尿樣中DNR的檢測。文中通過吸收光譜、熒光光譜的變化,并結(jié)合熒光壽命的測量和量子化學(xué)計(jì)算,對(duì)TPPS4與DNR相互作用的機(jī)理、兩者之間的作用力、復(fù)合物的組成與結(jié)構(gòu)以及熒光猝滅的類型和吸收光譜、熒光光譜變化的原因進(jìn)行了討論。 2.熒光光譜法研究美洛昔康與乙酸雙氧鈾的相互作用及其分析應(yīng)用 以乙酸雙氧鈾(UA)為探針,提出了熒光法測定美洛昔康(MLX)的新方法。在pH=7.2的Tris-HCl緩沖溶液中,MLX與UA激發(fā)態(tài)分子生成瞬時(shí)的激發(fā)態(tài)復(fù)合物,導(dǎo)致UA的熒光猝滅,并隨著MLX濃度的增大,UA的熒光猝滅值(△F)與MLX濃度在0.02～7.5mg·L-1呈良好的線性關(guān)系,檢出限為4.49ng-mL-1.實(shí)驗(yàn)研究了熒光猝滅反應(yīng)的適宜條件和影響因素,考察了共存物質(zhì)的影響,表明方法具有較好的選擇性,可用于美洛昔康片劑與膠囊中美洛昔康含量的測定。文中通過對(duì)吸收光譜、猝滅常數(shù)Kq以及溫度對(duì)熒光猝滅作用影響的討論,表明美洛昔康對(duì)乙酸雙氧鈾的熒光猝滅為動(dòng)態(tài)猝滅。 3.鄰菲羅啉熒光增強(qiáng)法測定鎬 在pH5.5的BR緩沖溶液中,Cd(Ⅱ)與鄰菲羅啉(phen)相互作用,導(dǎo)致反應(yīng)體系的熒光增強(qiáng),最大激發(fā)和最大發(fā)射波長分別為328nm和368nm.Cd(Ⅱ)濃度在0.4-21.0μg·mL-1范圍內(nèi)與體系熒光增強(qiáng)值(△F)呈良好的線性關(guān)系,檢出限為138.9ng-mL-1.實(shí)驗(yàn)研究了熒光增強(qiáng)反應(yīng)的適宜條件和影響因素,考察了共存物質(zhì)的影響,表明方法具有較好的選擇性,可用于環(huán)境水樣中Cd(Ⅱ)含量的測定。 4.赤蘚紅-鄰菲羅啉-鎘(Ⅱ)三元配合物的吸收與共振瑞利散射光譜研究及其分析應(yīng)用 在pH7.0-8.0的KH2PO4-Na2HPO4緩沖溶液中,Cd(Ⅱ)與鄰菲羅啉(phen)形成穩(wěn)定的陽離子螯合物,再進(jìn)一步與赤蘚紅(Ery)陰離子通過靜電引力和疏水作用力相互作用生成三元離子締合物。該締合反應(yīng)能引起體系吸收光譜的變化,發(fā)生明顯的褪色反應(yīng),且最大褪色波長位于528nm處。體系吸光度的減小值(△A)在一定范圍內(nèi)與Cd()濃度成正比,據(jù)此建立了測定鎘離子的高靈敏度的分光光度法,摩爾吸光系數(shù)ε528=2.29x105L-mol-1·cm1,檢出限為26.5ng-mL-1.此外,其還能引起散射光譜的改變。該反應(yīng)體系在371nm與590nm波長處均出現(xiàn)共振瑞利散射(RRS)明顯增強(qiáng)的現(xiàn)象,在640nm和350nm左右波長處出現(xiàn)二級(jí)散射(SOS)和倍頻散射(FDS)。在實(shí)驗(yàn)最佳條件下,散射增強(qiáng)值(ΔIRRS、ΔISOS和ΔIFDS)均在一定范圍內(nèi)與Cd(Ⅱ)濃度成良好的線性關(guān)系。散射方法均具有較高的靈敏度,對(duì)Cd(Ⅱ)的檢出限分別為1.27ng·mL-1(雙波長疊加法)、1.39ng·mL-1(RRS,371nm)、4.03ng·mL-1(RRS,590nm)、5.92ng·mL-1(SOS)和14.7ng·mL-1(FDS),且都可用于環(huán)境中痕量Cd(Ⅱ)的測定。本實(shí)驗(yàn)研究了反應(yīng)體系的RRS、SOS、FDS和吸收光譜特征與適宜的反應(yīng)條件和影響因素,并以RRS法為例考察了方法的選擇性。對(duì)于環(huán)境水樣中的Cd(Ⅱ)含量的測定,回收率在93.0%～103.0%范圍,相對(duì)標(biāo)準(zhǔn)偏差在2.5%～4.3%之間。測定結(jié)果與原子吸收分光光度法(AAS)對(duì)照,基本一致。
[Abstract]:The determination of daunorubicin, meloxicam and cadmium ions by fluorescence spectroscopy and Resonance Rayleigh scattering technique is mainly used to study their interaction with the probe meso- four (4- sulfonyl phenyl) porphyrin, uranyl acetate, phenanthroline and erythrin. The interaction of their interactions with the absorption spectrum and quantum chemical calculation is also discussed. In this way, a new method for the determination of daunorubicin, meloxicam and cadmium ions was established, and the experimental method was applied to the detection of actual samples. The main contents are as follows:
1. fluorescence quenching and spectrophotometric determination of daunorubicin with meso- four (4- sulfonyl phenyl) porphyrin as probe
A new method for the determination of daunorubicin hydrochloride (DNR) by fluorescence and absorption spectroscopy was proposed with the synthesis of meso- four (4- sulfonphenyl) porphyrin (TPPS4). In pH4.6's Potassium phthalate -NaOH buffer solution, TPPS4 and DNR interact with the electrostatic force and hydrophobic forces to form a binding product of 1:1, resulting in the fluorescence quenching of TPPS4. The fluorescence intensity of the system was detected at the maximum excitation wavelength (lambda Ex) and the maximum emission wavelength (lambda EM) (lambda ex/ lambda em=435nm/672nm). The experimental results showed that the fluorescence quenching value of TPPS4 (AF) had a good linear relationship with the DNR concentration from 0.8 to 6.0mg. L-1, and the detection limit was 27.0ng. ML-1., and the absorbance of the system gradually weakened in the 433nm. A new absorption peak was found at 420nm, and the two absorbance change value (AA) followed the ear law in a certain range with the concentration of DNR. The molar absorption coefficient (epsilon) was epsilon 433=7.75x104L. Mol-1 cm-1 (Discoloration method), epsilon 420=5.19 x 104L. Mol-1 cm-1 (color adding method). When the double wavelength superposition method was used, the molar absorption coefficient could reach 1.29 x 105L. Mol-1. 1. the suitable conditions and influencing factors of fluorescence quenching reaction were studied and the influence of coexistent substances was investigated. The results showed that the method had good selectivity and was suitable for the detection of DNR in blood samples and urine samples. The interaction between TPPS4 and DNR was used by the absorption spectrum, the change of fluorescence spectrum, the measurement of fluorescence lifetime and the quantum chemical calculation. The mechanism, the interaction between the two, the composition and structure of the complex, the types of fluorescence quenching, the absorption spectra and the reasons for the fluorescence spectra changes were discussed.
2. fluorescence spectroscopy study of the interaction between meloxicam and uranyl acetate and Its Analytical Application
A new method for the determination of meloxicam (MLX) by fluorimetric method was proposed with UA as a probe. In the Tris-HCl buffer solution of pH=7.2, the transient excited state complex of MLX and UA excited states was produced, which resulted in the fluorescence quenching of UA. As the concentration of MLX increased, the fluorescence quenching value of UA (delta F) was in good condition with MLX concentration from 0.02 to 7.5mg. The optimum conditions and influencing factors of fluorescence quenching reaction were studied by 4.49ng-mL-1. test, and the effect of coexistent substances was investigated. The results showed that the method had good selectivity and could be used for the determination of meloxicam content in meloxicam tablets and capsules. The absorption spectrum, quenching constant Kq and temperature to fluorescein were used in this paper. The discussion of the effect of photoquenching shows that meloxicam is a dynamic quenching for the fluorescence quenching of uranyl acetate.
Determination of pickaxe by 3. ortho phenanthroline fluorescence enhancement
In the BR buffer solution of pH5.5, the interaction of Cd (II) with adjacent phenanthroline (phen) leads to the enhancement of the fluorescence of the reaction system. The maximum excitation and maximum emission wavelengths are 328nm and 368nm.Cd (II), respectively, in the 0.4-21.0 mu g / mL-1 range, which have a good linear relationship with the fluorescence enhancement value (delta F) of the system. The detection limit is a 138.9ng-mL-1. experimental study. The suitable conditions and influencing factors of the fluorescence enhanced reaction were studied, and the influence of the coexisting substances was investigated. The results showed that the method had good selectivity and could be used for the determination of Cd (II) content in environmental water samples.
Absorption and Resonance Rayleigh scattering spectra of 4. erythrin red phenanthroline cadmium (II) three complexes and their analytical applications
In the KH2PO4-Na2HPO4 buffer solution of pH7.0-8.0, Cd (II) forms a stable cation chelate with adjacent phenanthroline (phen), and further produces a three element ion association with the interaction of Ery anions through electrostatic and hydrophobic forces. The association reaction can cause changes in the absorption spectrum of the system, and a distinct fading reaction occurs. The maximum fading wavelength of the system is located at 528nm. The reduced value of the system absorbance (delta A) is proportional to the concentration of Cd () in a certain range. According to this, a high sensitivity spectrophotometric method for the determination of cadmium ions is established. The molar absorption coefficient is 528=2.29x105L-mol-1. CM1, the detection limit is 26.5ng-mL-1., which can also cause the change of the scattering spectrum. The resonance Rayleigh scattering (RRS) is obviously enhanced at the wavelength of 371nm and 590nm, and two stages of scattering (SOS) and frequency doubling scattering (FDS) appear at the wavelength of 640nm and 350nm. The scattering enhancement (delta IRRS, Delta ISOS and delta IFDS) is in a good linear relationship with Cd (II) concentration in a certain range of experimental conditions. The detection limits for Cd (II) are 1.27ng. ML-1 (double wavelength superposition), 1.39ng. ML-1 (RRS, 371nm), 4.03ng. ML-1 (RRS, 590nm), 5.92ng. The reaction conditions and influencing factors are suitable and the selectivity of the method is examined by the RRS method. The recovery rate of the Cd (II) content in the environmental water samples is from 93% to 103%, the relative standard deviation is between 2.5% and 4.3%. The results are compared with the atomic absorption spectrophotometry (AAS), basically the same.
【學(xué)位授予單位】：西南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：O657.3;R927
本文編號(hào)：2157869
[Abstract]:The determination of daunorubicin, meloxicam and cadmium ions by fluorescence spectroscopy and Resonance Rayleigh scattering technique is mainly used to study their interaction with the probe meso- four (4- sulfonyl phenyl) porphyrin, uranyl acetate, phenanthroline and erythrin. The interaction of their interactions with the absorption spectrum and quantum chemical calculation is also discussed. In this way, a new method for the determination of daunorubicin, meloxicam and cadmium ions was established, and the experimental method was applied to the detection of actual samples. The main contents are as follows:
1. fluorescence quenching and spectrophotometric determination of daunorubicin with meso- four (4- sulfonyl phenyl) porphyrin as probe
A new method for the determination of daunorubicin hydrochloride (DNR) by fluorescence and absorption spectroscopy was proposed with the synthesis of meso- four (4- sulfonphenyl) porphyrin (TPPS4). In pH4.6's Potassium phthalate -NaOH buffer solution, TPPS4 and DNR interact with the electrostatic force and hydrophobic forces to form a binding product of 1:1, resulting in the fluorescence quenching of TPPS4. The fluorescence intensity of the system was detected at the maximum excitation wavelength (lambda Ex) and the maximum emission wavelength (lambda EM) (lambda ex/ lambda em=435nm/672nm). The experimental results showed that the fluorescence quenching value of TPPS4 (AF) had a good linear relationship with the DNR concentration from 0.8 to 6.0mg. L-1, and the detection limit was 27.0ng. ML-1., and the absorbance of the system gradually weakened in the 433nm. A new absorption peak was found at 420nm, and the two absorbance change value (AA) followed the ear law in a certain range with the concentration of DNR. The molar absorption coefficient (epsilon) was epsilon 433=7.75x104L. Mol-1 cm-1 (Discoloration method), epsilon 420=5.19 x 104L. Mol-1 cm-1 (color adding method). When the double wavelength superposition method was used, the molar absorption coefficient could reach 1.29 x 105L. Mol-1. 1. the suitable conditions and influencing factors of fluorescence quenching reaction were studied and the influence of coexistent substances was investigated. The results showed that the method had good selectivity and was suitable for the detection of DNR in blood samples and urine samples. The interaction between TPPS4 and DNR was used by the absorption spectrum, the change of fluorescence spectrum, the measurement of fluorescence lifetime and the quantum chemical calculation. The mechanism, the interaction between the two, the composition and structure of the complex, the types of fluorescence quenching, the absorption spectra and the reasons for the fluorescence spectra changes were discussed.
2. fluorescence spectroscopy study of the interaction between meloxicam and uranyl acetate and Its Analytical Application
A new method for the determination of meloxicam (MLX) by fluorimetric method was proposed with UA as a probe. In the Tris-HCl buffer solution of pH=7.2, the transient excited state complex of MLX and UA excited states was produced, which resulted in the fluorescence quenching of UA. As the concentration of MLX increased, the fluorescence quenching value of UA (delta F) was in good condition with MLX concentration from 0.02 to 7.5mg. The optimum conditions and influencing factors of fluorescence quenching reaction were studied by 4.49ng-mL-1. test, and the effect of coexistent substances was investigated. The results showed that the method had good selectivity and could be used for the determination of meloxicam content in meloxicam tablets and capsules. The absorption spectrum, quenching constant Kq and temperature to fluorescein were used in this paper. The discussion of the effect of photoquenching shows that meloxicam is a dynamic quenching for the fluorescence quenching of uranyl acetate.
Determination of pickaxe by 3. ortho phenanthroline fluorescence enhancement
In the BR buffer solution of pH5.5, the interaction of Cd (II) with adjacent phenanthroline (phen) leads to the enhancement of the fluorescence of the reaction system. The maximum excitation and maximum emission wavelengths are 328nm and 368nm.Cd (II), respectively, in the 0.4-21.0 mu g / mL-1 range, which have a good linear relationship with the fluorescence enhancement value (delta F) of the system. The detection limit is a 138.9ng-mL-1. experimental study. The suitable conditions and influencing factors of the fluorescence enhanced reaction were studied, and the influence of the coexisting substances was investigated. The results showed that the method had good selectivity and could be used for the determination of Cd (II) content in environmental water samples.
Absorption and Resonance Rayleigh scattering spectra of 4. erythrin red phenanthroline cadmium (II) three complexes and their analytical applications
In the KH2PO4-Na2HPO4 buffer solution of pH7.0-8.0, Cd (II) forms a stable cation chelate with adjacent phenanthroline (phen), and further produces a three element ion association with the interaction of Ery anions through electrostatic and hydrophobic forces. The association reaction can cause changes in the absorption spectrum of the system, and a distinct fading reaction occurs. The maximum fading wavelength of the system is located at 528nm. The reduced value of the system absorbance (delta A) is proportional to the concentration of Cd () in a certain range. According to this, a high sensitivity spectrophotometric method for the determination of cadmium ions is established. The molar absorption coefficient is 528=2.29x105L-mol-1. CM1, the detection limit is 26.5ng-mL-1., which can also cause the change of the scattering spectrum. The resonance Rayleigh scattering (RRS) is obviously enhanced at the wavelength of 371nm and 590nm, and two stages of scattering (SOS) and frequency doubling scattering (FDS) appear at the wavelength of 640nm and 350nm. The scattering enhancement (delta IRRS, Delta ISOS and delta IFDS) is in a good linear relationship with Cd (II) concentration in a certain range of experimental conditions. The detection limits for Cd (II) are 1.27ng. ML-1 (double wavelength superposition), 1.39ng. ML-1 (RRS, 371nm), 4.03ng. ML-1 (RRS, 590nm), 5.92ng. The reaction conditions and influencing factors are suitable and the selectivity of the method is examined by the RRS method. The recovery rate of the Cd (II) content in the environmental water samples is from 93% to 103%, the relative standard deviation is between 2.5% and 4.3%. The results are compared with the atomic absorption spectrophotometry (AAS), basically the same.
【學(xué)位授予單位】：西南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：O657.3;R927
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