CN101241076A - A kind of assay method of hydroxyl free radical concentration - Google Patents
A kind of assay method of hydroxyl free radical concentration Download PDFInfo
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- -1 hydroxyl free radical Chemical class 0.000 title claims description 39
- 238000003556 assay Methods 0.000 title claims description 8
- CDOWNLMZVKJRSC-UHFFFAOYSA-N 2-hydroxyterephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(O)=C1 CDOWNLMZVKJRSC-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 19
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- VIQSRHWJEKERKR-UHFFFAOYSA-L disodium;terephthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 VIQSRHWJEKERKR-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 19
- 239000012086 standard solution Substances 0.000 claims description 11
- 238000002284 excitation--emission spectrum Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000012064 sodium phosphate buffer Substances 0.000 claims description 5
- 238000002798 spectrophotometry method Methods 0.000 claims description 5
- 238000002189 fluorescence spectrum Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- HQWKKEIVHQXCPI-UHFFFAOYSA-L disodium;phthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C([O-])=O HQWKKEIVHQXCPI-UHFFFAOYSA-L 0.000 claims 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 2
- 241001602876 Nata Species 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000000804 electron spin resonance spectroscopy Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 238000007262 aromatic hydroxylation reaction Methods 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- IISLNQNUYOZKNE-UHFFFAOYSA-N sodium;terephthalic acid Chemical compound [Na].OC(=O)C1=CC=C(C(O)=O)C=C1 IISLNQNUYOZKNE-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
一种羟基自由基浓度的测定方法，将捕获剂对苯二甲酸钠盐(NaTA)加入羟基自由基产生的体系中，对苯二甲酸纳盐与体系中所产生的羟基自由基反应生成2－羟基对苯二甲酸(HTA)，2－羟基对苯二甲酸具有稳定的荧光性，使用荧光分光光度计测定(激发波长λex＝315nm，发射波长λem＝425nm)，然后再将测得的2－羟基对苯二甲酸浓度换算成羟基自由基浓度。本测定方法易行、可靠、准确，对于在羟基自由基产生体系的环境pH＜12，或羟基自由基产生体系的溶液对电导率有要求的情况下本发明尤其适用。A method for measuring the concentration of hydroxyl radicals. The capture agent sodium terephthalate (NaTA) is added to a system generating hydroxyl radicals, and the sodium terephthalate reacts with the hydroxyl radicals generated in the system to generate 2-hydroxyl radicals. Terephthalic acid (HTA), 2-hydroxyterephthalic acid has stable fluorescence, which is measured by a fluorescence spectrophotometer (excitation wavelength λ ex =315nm, emission wavelength λ em =425nm), and then the measured 2 - Convert the concentration of hydroxyterephthalic acid into the concentration of hydroxyl radicals. The measuring method is easy, reliable and accurate, and is especially suitable for the case where the environment pH of the hydroxyl radical generating system is less than 12, or the solution of the hydroxyl radical generating system requires conductivity.
Description
技术领域technical field
本发明涉及一种羟基自由基的测定方法，使用对苯二甲酸钠盐作为羟基自由基捕获剂，生成2-羟基对苯二甲酸，然后利用荧光分光光度计法间接测定羟基自由基。The invention relates to a method for measuring hydroxyl radicals, which uses sodium terephthalate as a hydroxyl radical scavenger to generate 2-hydroxyterephthalic acid, and then uses a fluorescence spectrophotometer to indirectly measure hydroxyl radicals.
背景技术Background technique
由于羟基自由基为极其活泼的物质，它与大部分化合物反应的速率非常快使得它的存在寿命在10-9s数量级，所以对羟基自由基的测定非常困难，也是科学界研究热点。Since hydroxyl radical is an extremely active substance, its reaction rate with most compounds is very fast so that its lifetime is on the order of 10 -9 s, so the determination of hydroxyl radical is very difficult, and it is also a research hotspot in the scientific community.
目前国内外关于羟基自由基测定的文献非常多，主要分为直接测定和间接测定。At present, there are many literatures on the determination of hydroxyl radicals at home and abroad, which are mainly divided into direct determination and indirect determination.
直接测定方法主要有以电子自旋共振能谱法(ESR)为代表，但是这种方法的缺点是灵敏度不够，而且不能定量测定羟基自由基。另外直接测定法所需要的仪器都是非常昂贵的，一般实验室无法满足要求。The direct determination method is mainly represented by electron spin resonance spectroscopy (ESR), but the disadvantage of this method is that the sensitivity is not enough, and the hydroxyl radical cannot be quantitatively determined. In addition, the instruments required for direct determination are very expensive, and general laboratories cannot meet the requirements.
间接测定方法是指芳族羟基化，主要原理：用芳族化合物(苯酚、苯甲酸、水杨酸等)作为捕获剂与羟基自由基反应，生成相对稳定的羟基化产物，然后使用各种手段测定相对稳定的羟基化产物，从而间接测定羟基自由基。间接测定法由于其捕获剂的选择目前尚未统一，同时存在着降低测定成本的可能性，所以迅速成为研究的热点。The indirect determination method refers to aromatic hydroxylation, the main principle: use aromatic compounds (phenol, benzoic acid, salicylic acid, etc.) Determination of relatively stable hydroxylated products, thereby indirect determination of hydroxyl radicals. Indirect assay has become a research hotspot rapidly because the selection of its capture agent has not been unified yet, and there is a possibility of reducing the cost of assay.
国外对于羟基自由基间接测定法产生的羟基化产物测定主要依靠高效液相色谱、气相色谱等仪器，国内则使用分光光度计法测定羟基自由基的文献比较多。间接测定法由于所选的捕获剂与羟基自由基反应的机理非常复杂，影响测定准确度的因素非常多。捕获剂与羟基自由基反应途径是否唯一，反应之后的羟基化产物是否稳定，都是有待确定的。In foreign countries, the determination of hydroxylated products produced by the indirect determination of hydroxyl radicals mainly relies on high-performance liquid chromatography, gas chromatography and other instruments, while there are many domestic literatures on the use of spectrophotometers to measure hydroxyl radicals. Due to the complex reaction mechanism of the selected capture agent and hydroxyl radicals in the indirect assay method, there are many factors that affect the accuracy of the assay. It remains to be determined whether the reaction pathway between the capture agent and the hydroxyl radical is unique, and whether the hydroxylated product after the reaction is stable.
中国发明专利公开了两种羟基自由基测定方法(CN1412553和CN101042371)，分别使用异丙醇和对羟基苯甲酸为捕获剂，由于机理复杂、影响测定准确度的因素多而易造成系统误差；对于中间产物的测定，气相色谱精确度高但操作较为烦琐，而通过响应电流电位测定操作简单但精确度则稍差。Chinese invention patent discloses two kinds of hydroxyl radical assay methods (CN1412553 and CN101042371), use isopropanol and p-hydroxybenzoic acid respectively as capture agent, because mechanism is complicated, the factor that affects measurement accuracy is many and easily causes systematic error; For intermediate For the determination of products, gas chromatography has high precision but the operation is more cumbersome, while the measurement by response current potential is simple but less accurate.
羟基自由基广泛应用使得其浓度测定方法的研究成为热点，羟基自由基浓度测定方法的准确度的提高和成本的降低将是未来研究的趋势。The wide application of hydroxyl radicals makes the research of its concentration determination method become a hotspot, and the improvement of the accuracy and cost reduction of the concentration determination method of hydroxyl radicals will be the trend of future research.
发明内容Contents of the invention
本发明目的是提供一种羟基自由基的测定方法，使用对苯二甲酸钠盐作为捕获剂，用以克服对苯二甲酸作为捕获剂时只能在强碱条件下溶解的局限。对于在羟基自由基产生体系的环境pH＜12，或羟基自由基产生体系的溶液对电导率有要求(如：液中脉冲放电产生羟基自由基体系)的情况下本测定方法尤其适用。使用荧光分光光度法，根据波峰面积测定的2-羟基对苯二甲酸浓度，最后换算成羟基自由基浓度，本测定方法易行、可靠、准确。The purpose of the present invention is to provide a method for measuring hydroxyl radicals, using sodium terephthalate as a trapping agent to overcome the limitation that terephthalic acid can only be dissolved under strong alkali conditions as a trapping agent. This determination method is especially suitable for the case where the environment pH of the hydroxyl radical generating system is less than 12, or the solution of the hydroxyl radical generating system has a requirement for conductivity (for example, a pulse discharge in liquid generates a hydroxyl radical system). Fluorescence spectrophotometry is used to measure the concentration of 2-hydroxyterephthalic acid according to the peak area, and finally converted into the concentration of hydroxyl radicals. The determination method is easy, reliable and accurate.
本发明的技术方案是：配制2-羟基对苯二甲酸标准溶液，用荧光分光光度计测定各标准溶液的光谱图，得到2-羟基对苯二甲酸标准溶液浓度和光谱图面积对应关系的标准曲线；实际测定时将捕获剂对苯二甲酸钠盐过量加入羟基自由基产生的体系中，与体系中产生的羟基自由基反应生成2-羟基对苯二甲酸，采用荧光分光光度计检测混合溶液，得到激发-发射光谱特征图；最后，根据特征图给出的波峰面积，通过波峰面积与2-羟基对苯二甲酸摩尔浓度关系的标准曲线，得到此波峰面积下对应的2-羟基对苯二甲酸摩尔浓度，再由化学反应关系式得到的换算公式换算出羟基自由基的摩尔浓度。The technical scheme of the present invention is: prepare 2-hydroxyterephthalic acid standard solution, measure the spectrogram of each standard solution with a fluorescence spectrophotometer, obtain the standard of the corresponding relationship between the concentration of 2-hydroxyterephthalic acid standard solution and the area of the spectrogram Curve; during the actual measurement, the capture agent sodium terephthalate was added excessively to the system generated by hydroxyl radicals, and reacted with the hydroxyl radicals generated in the system to generate 2-hydroxyterephthalic acid, and the mixed solution was detected by a fluorescence spectrophotometer. Obtain the characteristic figure of excitation-emission spectrum; Finally, according to the peak area that characteristic figure provides, by the standard curve of peak area and 2-hydroxyterephthalic acid molar concentration relation, obtain the corresponding 2-hydroxyterephthalic acid under this peak area The molar concentration of formic acid is converted to the molar concentration of hydroxyl radicals by the conversion formula obtained from the chemical reaction relational formula.
上述测定方法测定过程中，对苯二甲酸钠盐与羟基自由基反应的体系中要通入O2，通入时间为30min，此时反应体系下的溶液达到氧饱和；采用荧光分光光度计检测之前使用磷酸钠(0.2M，pH＝7.4)缓冲溶液调节pH值在6～11范围内。During the measurement process of the above-mentioned determination method, O2 should be introduced into the reaction system of sodium terephthalate and hydroxyl radicals for 30 minutes. At this time, the solution under the reaction system reaches oxygen saturation; Sodium phosphate (0.2M, pH=7.4) buffer solution was used to adjust the pH value in the range of 6-11.
上述荧光分光光度法检测时，使用波长315nm的荧光进行激发，在340～625nm波长范围收集样品的荧光光谱。During the detection by the above-mentioned fluorescence spectrophotometry, fluorescence with a wavelength of 315 nm is used for excitation, and the fluorescence spectrum of the sample is collected in the wavelength range of 340-625 nm.
本发明利用捕获剂与羟基自由基反应，通过测定反应的中间产物浓度间接测定羟基自由基。对苯二甲酸钠盐捕获羟基自由基产生2-羟基对苯二甲酸的反应途径如下：The invention utilizes the capture agent to react with the hydroxyl free radical, and indirectly measures the hydroxyl free radical by measuring the concentration of the intermediate product of the reaction. The reaction route that terephthalic acid sodium salt captures hydroxyl radical to produce 2-hydroxy terephthalic acid is as follows:
根据对苯二甲酸钠盐捕获羟基自由基反应原理的研究，在体系中溶氧饱和时，捕获反应的效率为35％，即已知2-羟基对苯二甲酸的摩尔浓度，可以根据下式计算羟基自由基浓度：According to the research on the reaction principle of the sodium terephthalic acid to capture hydroxyl radicals, when the dissolved oxygen in the system is saturated, the efficiency of the capture reaction is 35%, that is, the known molar concentration of 2-hydroxyterephthalic acid can be calculated according to the following formula Hydroxyl radical concentration:
式中：COH·为羟基自由基浓度，M；In the formula: C OH is the concentration of hydroxyl radicals, M;
C2-羟基对苯二甲酸为2-羟基对苯二甲酸浓度，MC 2-hydroxyterephthalic acid is the concentration of 2-hydroxyterephthalic acid, M
使用荧光分光光度法测定2-羟基对苯二甲酸浓度，通过上述公式，间接求出羟基自由基浓度。The concentration of 2-hydroxyterephthalic acid was measured by fluorescence spectrophotometry, and the concentration of hydroxyl radicals was obtained indirectly by the above formula.
本发明使用的捕获剂与羟基自由基反应的中间产物2-羟基对苯二甲酸在0～2.0×10-3M浓度范围对荧光光谱波峰面积有线性响应关系，所以本发明羟基自由基检测范围为0～5.7×10-3M。2-羟基对苯二甲酸在5.0×10-7M浓度时可检出荧光光谱，即本发明最低检测限为1.5×10-6M。The intermediate product 2-hydroxyterephthalic acid in the reaction between the capture agent used in the present invention and hydroxyl radicals has a linear response relationship to the peak area of the fluorescence spectrum in the concentration range of 0 to 2.0×10 -3 M, so the detection range of hydroxyl radicals in the present invention is 0 to 5.7×10 -3 M. The fluorescence spectrum can be detected at the concentration of 2-hydroxyterephthalic acid at 5.0×10 -7 M, that is, the minimum detection limit of the present invention is 1.5×10 -6 M.
具体实施方式Detailed ways
本发明测定羟基自由基浓度的主要步骤如下：The main steps of the present invention's determination of hydroxyl radical concentration are as follows:
1.绘制标准曲线1. Draw a standard curve
(1)配制0～2.0×10-3M范围内的一系列捕获产物2-羟基对苯二甲酸标准溶液，建议取6个标准浓度：0M、0.2×10-3M、0.5×10-3M、1.0×10-3M、1.5×10-3M、2.0×10-3M。(1) Prepare a series of standard solutions of capture product 2-hydroxyterephthalic acid in the range of 0～2.0×10 -3 M. It is recommended to take 6 standard concentrations: 0M, 0.2×10 -3 M, 0.5×10 -3 M, 1.0×10 -3 M, 1.5×10 -3 M, 2.0×10 -3 M.
(2)每次取5.00ml标准溶液，加入5.00ml磷酸钠缓冲溶液，用荧光分光光度法测定，计算激发—发射光谱特征图的波峰面积；(2) get 5.00ml standard solution at every turn, add 5.00ml sodium phosphate buffer solution, measure with fluorescence spectrophotometry, calculate the peak area of excitation-emission spectrum characteristic figure;
(3)以测得的激发—发射光谱特征图的波峰面积为纵坐标，以2-羟基对苯二甲酸标准溶液浓度为横坐标，绘制标准曲线；(3) taking the peak area of the excitation-emission spectrum characteristic figure as the ordinate, and taking the concentration of the 2-hydroxyterephthalic acid standard solution as the abscissa, draw a calibration curve;
2.测定2-羟基对苯二甲酸浓度2. Determination of 2-hydroxyterephthalic acid concentration
向被测体系中通入氧气直到氧饱和，以过量的对苯二甲酸钠盐为捕获剂，反应时间20～30min，取出5.00ml反应溶液依照步骤1中(1)进行荧光法分析，使用波长315nm进行激发，在340～625nm波长范围收集样品的荧光发生光谱，得到激发—发射光谱特征图的波峰面积；由测得的水样的激发—发射光谱特征图的波峰面积和步骤1中(3)绘制的标准曲线得到溶液中2-羟基对苯二甲酸摩尔浓度。Introduce oxygen into the system to be tested until oxygen saturation, use excess sodium terephthalate as a capture agent, and take out 5.00ml of the reaction solution for 20-30min reaction time, and perform fluorescence analysis according to (1) in step 1, using a wavelength of 315nm Excite, collect the fluorescence generation spectrum of the sample in the 340-625nm wavelength range, and obtain the peak area of the excitation-emission spectrum characteristic map; The drawn standard curve obtained the molar concentration of 2-hydroxyterephthalic acid in the solution.
3.通过公式计算出羟基自由基摩尔浓度。3. Through the formula Calculate the molar concentration of hydroxyl radicals.
实施例Example
对液中高压脉冲放电体系生成的羟基自由基浓度进行测定。用蒸馏水在烧杯中配置5×10-4M浓度的对苯二甲酸钠溶液1L，使用磁力搅拌器搅拌，过夜，待用。使用0.1mol/L的NaCl溶液调节溶液电导率到150μs/cm。将配置好的溶液置于液中高压脉冲放电装置的反应容器中，以400ml/min的流量向反应器中通入O2，10min之后启动系统电源，峰值电压60kV，反应之后15min和30min各取5.00ml反应溶液一次，加入pH＝7.4的磷酸钠缓冲溶液5.00ml。使用荧光分光光度计测定溶液荧光性，计算激发—发射光谱特征图的波峰面积，通过绘制的标准曲线对2-羟基对苯二甲酸进行定量分析。结果：通电15min后，溶液羟基自由基浓度为2.57×10-5M，通电30min后，溶液羟基自由基浓度为4.96×10-5M。The concentration of hydroxyl radicals generated by the high-voltage pulse discharge system in the liquid was measured. Prepare 1 L of sodium terephthalate solution with a concentration of 5×10 −4 M in a beaker with distilled water, stir it with a magnetic stirrer overnight, and set it aside for use. Use 0.1mol/L NaCl solution to adjust the conductivity of the solution to 150μs/cm. Put the prepared solution in the reaction container of the high-voltage pulse discharge device in the liquid, feed O 2 into the reactor at a flow rate of 400ml/min, start the system power after 10 minutes, the peak voltage is 60kV, and take 15 minutes and 30 minutes after the reaction. 5.00 ml of the reaction solution was added once, and 5.00 ml of sodium phosphate buffer solution with pH=7.4 was added. Fluorescence of the solution was measured by a fluorescence spectrophotometer, the peak area of the excitation-emission spectrum characteristic map was calculated, and the quantitative analysis of 2-hydroxyterephthalic acid was carried out through the drawn standard curve. Results: After electrifying for 15 minutes, the concentration of hydroxyl radicals in the solution was 2.57×10 -5 M, and after electrifying for 30 minutes, the concentration of hydroxyl radicals in the solution was 4.96×10 -5 M.
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