基质固相分散—高效液相色谱—串联质谱检测印染污泥中的染料类污染物
发布时间：2018-11-22 14:28
【摘要】：印染行业是国民经济重要支柱产业之一,行业所需的原料——染料是工业和生活中必不可少的原材料。染料的种类繁多,其中一些染料中含有对环境和人体有害的物质,许多国家和相关组织对这些染料的使用作出严格的限制。部分分散染料和酸性染料对人体有致敏作用,能引起人体皮肤、黏膜或呼吸道过敏,有的还具有致癌性、致突变等毒性作用。生产排放的染料类污染物通过印染废水积聚到印染污泥中,往往成为很难处理的一类污染物。染料中的有害成分通过污泥的循环利用转移到环境中,使得人体和动植物的健康受到潜在的威胁。因此,对于印染污泥中染料类污染物的检测显得尤为重要,但是印染污泥成分复杂,要分析其中的染料类污染物存在相当大的难度,所以选择符合要求的样品前处理方法和检测方法很关键。基质固相分散(Matrix Solid-Phase Dispersion,MSPD)技术操作快速简便,所需溶剂和样品量少,特别适合于粘性样品(例如生物组织)、固体、半固体的处理。MSPD技术自发明以来,其与GC-MS、HPLC-MS等相结合,在环境、医药卫生、食品等方面得到了广泛的应用。本文将MSPD技术应用于萃取污泥样品中的染料类污染物,提取液进入高效液相色谱-质谱联用(HPLC-MS/MS)检测,进行研究。本文主要有以下几点:1.介绍了染料类污染物的基本情况、常用于污泥样品的前处理方法及各自特点,着重说明基质固相分散萃取技术在各类样品中的应用。2.建立了基质固相分散-高效液相色谱-串联质谱法测定印染污泥中三种分散染料(分散蓝35、分散红1、分散橙37)的分析方法。优化了萃取剂的选择及用量、洗脱剂的选择及用量、研磨条件、净化剂条件等萃取效果的影响因素。三种分散染料在最优条件下,2～100μg/kg范围内线性关系良好(r20.998),检出限为0.01～0.14μg/kg。相对标准偏差2.9%～8.2%,加标回收率86.4%～106.4%,能满足印染污泥中痕量分散染料的同时检测。3.对MSPD萃取方法进行再次的试验,仍运用基质固相分散-高效液相色谱-串联质谱法测定印染污泥中四种酸性染料(酸性红1、酸性红87、酸性橙7和酸性蓝83)。四种酸性染料在最优条件下在5～100μg/kg范围内线性关系良好(r20.996),检出限为0.19～0.75μg/kg。加标回收率在81.7%～103.1%之间,相对标准偏差在1.3%～8.9%之间,能够同时满足污泥中酸性染料类污染物的分析测定。4.最后对实验进行总结,基质固相分散萃取设备简单,成本低廉,所需时间短,将其应用于污泥这种基质中的样品提取,发展潜力良好。
[Abstract]:Printing and dyeing industry is one of the important pillar industries of national economy. There are many kinds of dyes, some of which contain harmful substances to the environment and human body. Many countries and related organizations impose strict restrictions on the use of these dyes. Some disperse dyes and acid dyes can sensitize human body and cause skin, mucosal or respiratory allergies. Some of them have carcinogenic and mutagenic effects. The dye pollutants discharged from production are accumulated into the printing and dyeing sludge through printing and dyeing wastewater, which often become a class of pollutants that are difficult to deal with. The harmful components of dyes are transferred to the environment through the recycling of sludge, which makes the health of human body, animal and plant under potential threat. Therefore, the detection of dye pollutants in printing and dyeing sludge is particularly important, but the composition of printing and dyeing sludge is very complex, so it is very difficult to analyze the dye pollutants in printing and dyeing sludge. Therefore, it is very important to select sample pretreatment and detection methods that meet the requirements. Matrix solid dispersion (Matrix Solid-Phase Dispersion,MSPD) is a rapid and simple technique with less solvent and sample quantity. It is especially suitable for the treatment of viscous samples (such as biological tissue), solids and semisolids. Since the invention of MSPD technology, it has been combined with GC-MS,. HPLC-MS has been widely used in environment, medicine, food and so on. In this paper, MSPD technique was applied to extract dye pollutants from sludge samples, and the extract was detected by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). This paper has the following main points: 1. This paper introduces the basic situation of dye pollutants, the pretreatment methods and their characteristics of sludge samples, and emphatically explains the application of matrix solid phase dispersion extraction technology in all kinds of samples. 2. A method for the determination of three disperse dyes (disperse blue 35, disperse red 1, disperse orange 37) in printing and dyeing sludge by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry was established. The factors affecting the extraction effect were optimized, such as the selection and dosage of extractant, the selection and dosage of eluent, the grinding condition and the condition of purifying agent. Under the optimum conditions, the linear relationship between the three disperse dyes was good in the range of 100 渭 g/kg (r20.998), and the detection limit was 0.01 渭 g / kg. The relative standard deviation of 2.9and 8.2and the recovery rate of 86.4and 106.4can meet the requirement of simultaneous determination of trace disperse dyes in printing and dyeing sludge. The extraction method of MSPD was tested again, and four kinds of acid dyes (acid red 1, acid red 87, acid orange 7 and acid blue 83) in printing and dyeing sludge were determined by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry. The linear range of the four acid dyes is 5 渭 g/kg (r20.996), and the detection limit is 0.19 ~ 0.75 渭 g / kg 路kg ~ (-1) 路min ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). The recovery rate was between 81.7% and 103.1%, and the relative standard deviation was between 1.3% and 8.9%. Finally, the experimental results show that the matrix solid phase dispersion extraction equipment is simple, low cost and short time. It has a good development potential when it is applied to the sample extraction of sludge.
【学位授予单位】：苏州科技学院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：X832;O657.63
[Abstract]:Printing and dyeing industry is one of the important pillar industries of national economy. There are many kinds of dyes, some of which contain harmful substances to the environment and human body. Many countries and related organizations impose strict restrictions on the use of these dyes. Some disperse dyes and acid dyes can sensitize human body and cause skin, mucosal or respiratory allergies. Some of them have carcinogenic and mutagenic effects. The dye pollutants discharged from production are accumulated into the printing and dyeing sludge through printing and dyeing wastewater, which often become a class of pollutants that are difficult to deal with. The harmful components of dyes are transferred to the environment through the recycling of sludge, which makes the health of human body, animal and plant under potential threat. Therefore, the detection of dye pollutants in printing and dyeing sludge is particularly important, but the composition of printing and dyeing sludge is very complex, so it is very difficult to analyze the dye pollutants in printing and dyeing sludge. Therefore, it is very important to select sample pretreatment and detection methods that meet the requirements. Matrix solid dispersion (Matrix Solid-Phase Dispersion,MSPD) is a rapid and simple technique with less solvent and sample quantity. It is especially suitable for the treatment of viscous samples (such as biological tissue), solids and semisolids. Since the invention of MSPD technology, it has been combined with GC-MS,. HPLC-MS has been widely used in environment, medicine, food and so on. In this paper, MSPD technique was applied to extract dye pollutants from sludge samples, and the extract was detected by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). This paper has the following main points: 1. This paper introduces the basic situation of dye pollutants, the pretreatment methods and their characteristics of sludge samples, and emphatically explains the application of matrix solid phase dispersion extraction technology in all kinds of samples. 2. A method for the determination of three disperse dyes (disperse blue 35, disperse red 1, disperse orange 37) in printing and dyeing sludge by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry was established. The factors affecting the extraction effect were optimized, such as the selection and dosage of extractant, the selection and dosage of eluent, the grinding condition and the condition of purifying agent. Under the optimum conditions, the linear relationship between the three disperse dyes was good in the range of 100 渭 g/kg (r20.998), and the detection limit was 0.01 渭 g / kg. The relative standard deviation of 2.9and 8.2and the recovery rate of 86.4and 106.4can meet the requirement of simultaneous determination of trace disperse dyes in printing and dyeing sludge. The extraction method of MSPD was tested again, and four kinds of acid dyes (acid red 1, acid red 87, acid orange 7 and acid blue 83) in printing and dyeing sludge were determined by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry. The linear range of the four acid dyes is 5 渭 g/kg (r20.996), and the detection limit is 0.19 ~ 0.75 渭 g / kg 路kg ~ (-1) 路min ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). The recovery rate was between 81.7% and 103.1%, and the relative standard deviation was between 1.3% and 8.9%. Finally, the experimental results show that the matrix solid phase dispersion extraction equipment is simple, low cost and short time. It has a good development potential when it is applied to the sample extraction of sludge.
【学位授予单位】：苏州科技学院
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：X832;O657.63
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