摘要
本文共分三章。
第一章:文献综述,概括了塑料包装材料中内分泌干扰素邻苯二甲酸酯类物质分析方法的现状和进展情况。对邻苯二甲酸酯类内分泌干扰素进行了简要介绍,详细总结了样品前处理和检测技术的发展情况,以及这些技术在对塑料包装材料中内分泌干扰素邻苯二甲酸酯类物质分析中的应用。
第二章:本文利用固相萃取-气相色谱法对塑料包装材料中的6种内分泌干扰素邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二丁基苄基酯(BBP)、邻苯二甲酸二(2-乙基已基)酯(DEHP)和邻苯二甲酸二正辛酯(DNOP)进行了分析方法研究。采用无水乙醇超声辅助提取样品,低温处理去除杂质,结合ENVI-18固相萃取技术净化提取液,以气相色谱-氢火焰离子化检测器测定其含量。各待测组分的检出限均小于0.04μg/mL,回收率在92.8~116.7%之间。相对标准偏差小于8.2%。
第三章:将分散液液微萃取(DLLME)与气相色谱-氢火焰离子化检测器(GC-FID)技术相结合,建立了一种简单快速测定塑料包装材料在酸性模拟体系(3%乙酸水溶液)中六种邻苯二甲酸酯(PAEs)溶出的新方法。采用四氯化碳作萃取剂,乙腈为分散剂,在优化条件下,六种PAEs在1.0~100.0μg/L浓度范围内呈良好的线性关系,线性相关系数在0.9998~0.9999之间,检出限为0.15~1.5μg/L(S/N=3)。将本方法应用于塑料包装材料在酸性模拟体系下的邻苯二甲酸酯的分析检测,并且考察了自然放置时间,加热温度,加热时间对于塑料包装材料中PAEs溶出的影响,加标回收率72.9%~113.7%,相对标准偏差在1.9%~12.6%之间。
This thesis consists of four chapters.
In CHAPTER ONE, The current state and development of analytical methods of endocrine disruptors-phthalate esters in plastic packaging materials are summarized. Toxicity of phthalate esters is introduced briefly. The methods of sample pretreatment and phthalate esters determination are summarized systemically and these methods applied to analysis of phthalate esters as well.
In CHAPTER TWO, A determination method of six endocrine disruptors-phthalate esters in plastic packaging materials including Di-methylphthalate (DMP), Di-ethylphthalate (DEP), Dibutylphthalate (DBP), Butylbenzylphthalate (BBP), Di(2-ethylhexyl)p-hthalate (DEHP) and Di-n-octylphthalate (DNOP) is developed. These phthalate esters are analyzed by gas chromatography combined with solid phase extraction (SPE). The samples are prepared by ultrasonic-assisted extraction with ethanol. Then the extract is purified by removing impurity with low temperature treatment and SPE with ENVI-18 column. Finally the samples are analyzed by using gas chromatography with flame ionization detector (GC-FID). The limits of detection of the 6 pollutants were all below 0.04μg/mL. The average recoveries were between 92.8 and 116.7% with relative standard deviation (RSD) less than 8.2%.
In CHAPTER THREE, The effectual, rapid, simple and convenient method,dispersive liquid-liquid microextraction (DLLME) combination gas chromatography coupled with flame ionization detector(GC-FID), was used for the determination of six phthalate esters (PAEs) in acid simulative system(3% acetic acid liquid), Under the optimum extraction conditions (extraction solvent:carbon tetrachloride; dispersive solvent:acetonitrile), a good linear relationship was obtained in the range of 1.0~100.0μg/L, the correlation coefficients was 0.9998~0.9999 and the limits of detection was between 0.15~1.5μg/L (S/N=3). The PAEs of plastic packaging materials under acid simulative system condition was successfully analyzed by using the proposed method. The influencing factors of dissolving PAEs from plastic packaging materials, such as laying time laying time, heating temperature and heating time were researched. The recoveries, which had been spiked with different levels, fell in the range of 72.9%~113.7% and the relative standard deviations were between 1.9% and 12.6%.
引文
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