水中芳环化合物及氨基甲酸酯农药的液相色谱分析
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摘要
随着经济和社会的发展,水污染问题也日益突出,已成为社会各界关注的主要环境问题。其中,芳环化合物污染和农药残留超标是两个重要问题,对两类物质的监测尤为重要。本文第一章概括了芳环化合物和氨基甲酸酯农药的性质和危害,介绍了水环境中两类物质的主要分析方法。第二章,建立了液相色谱测定水中芳环化合物的方法。取代苯的测定采用盐析分相微萃取法,考察了萃取剂种类、盐析剂种类和加盐量等因素对萃取效果的影响,并优化了色谱条件。该方法线性相关良好,三组分相关系数(R)均在0.9999以上,邻氯苯酚、氯苯、乙苯的方法检出限(LODs)分别为0.07、0.2和9.0μg/L,加标回收率为71.7%-93.0 %,相对标准偏差(RSDs)为1.2%-5.2%。海水中多环芳烃和双酚A的测定采用自制微萃取瓶进行富集,考察了萃取剂种类和体积、萃取时间、盐度、pH值等参数对萃取效果的影响。多环芳烃在0.01-50 mg/L范围内线性良好,萘、菲和荧蒽的检出限为7.0-13.3 ng/L,加标回收率为92.6%-94.5%,相对标准偏差为0.9%-1.8%;双酚A线性范围为0.01-10 mg/L,相关系数0.9999,检出限为0.03μg/L,加标回收率为83.1%-86.5%,相对标准偏差小于6.5%。第三章建立了盐析分相微萃取-液相色谱法测定水中氨基甲酸酯农药的方法。异丁醇作萃取剂,硫酸铵作盐析剂,Diamonsil C18色谱柱分离,流动相为甲醇-水(体积比53:47),检测波长220nm。速灭威、呋喃丹和西维因呈现良好线性,方法检出限为0.4-5.7μg/L,加标回收率在78.6%-89.8%之间,相对标准偏差(RSD)小于5%。
With the development of economy and society, the water pollution has been the main environment problem and has been given more attention to the public. The pollution of aromatic compounds and pesticide residues are two important aspects, so it is necessary to monitor these two kinds of environmental pollutant. In the fisrt chapter, we summarized the characteristics and hazard of aromatic compounds and pesticide residues, and introduced the main analysis methods to these two kinds of pollutant. In the second chapter, new methods for separation and determination of the aromatic compounds by HPLC were established. Based on salting out phase separation microextraction and HPLC, a novel mothod was used for the determination of substituted benzenes in water samples. The types of extractant and inorganic salt, the extactant volume and saltinity were investigated. The methodology exhibited good linearity and the detection limits were 0.07μg/L for o-chlorophenol, 0.2μg/L for chlorobenzene and 9.0μg/L for ethylbenzene, respectively. The average recoveries and relative standard deviations were 71.7%-93.0% and 1.2%-5.2%, respectively. A simple and sensitive analytical method using microextraction flask coupled to HPLC has been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) and bisphenol A (BPA) in seawater. The impact of extractant, extractant volume, extraction time, salinity and pH value was investigated. For PAHs, the methodology exhibited good linearity between 0.01 to 50mg/L; the detection limits were 7.0-13.3ng/L; the average recoveries and relative standard deviations were 92.6%-94.5% and 0.9%-1.8%, respectively. For BPA, the methodology exhibited good linearity between 0.01 to 10 mg/L; the detection limit obtained by this method was 0.03μg/L; the recoveries of simulated seawater for 1.0 and 10.0μg/L were 86.5% and 83.1% with the relative standard deviations below 6%. In the last chapter, the method using salting out phase separation microextraction and HPLC was applied again for the determination of carbamate insecticides residues from water. Extraction solvent was iso-butyl alcohol and salting out agent was ammonium sulfate. A C18 column was used for separation with detection wavelength at 220nm; the mobile phase was a mixture of methanol and water (the ratio of volume was 53: 47). The detection limits were 0.4-5.7μg/L. The average recovery of pesticides ranged from 78.6% to 89.8% with the relative standard deviations below 5.0%.
With the development of economy and society, the water pollution has been the main environment problem and has been given more attention to the public. The pollution of aromatic compounds and pesticide residues are two important aspects, so it is necessary to monitor these two kinds of environmental pollutant. In the fisrt chapter, we summarized the characteristics and hazard of aromatic compounds and pesticide residues, and introduced the main analysis methods to these two kinds of pollutant. In the second chapter, new methods for separation and determination of the aromatic compounds by HPLC were established. Based on salting out phase separation microextraction and HPLC, a novel mothod was used for the determination of substituted benzenes in water samples. The types of extractant and inorganic salt, the extactant volume and saltinity were investigated. The methodology exhibited good linearity and the detection limits were 0.07μg/L for o-chlorophenol, 0.2μg/L for chlorobenzene and 9.0μg/L for ethylbenzene, respectively. The average recoveries and relative standard deviations were 71.7%-93.0% and 1.2%-5.2%, respectively. A simple and sensitive analytical method using microextraction flask coupled to HPLC has been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) and bisphenol A (BPA) in seawater. The impact of extractant, extractant volume, extraction time, salinity and pH value was investigated. For PAHs, the methodology exhibited good linearity between 0.01 to 50mg/L; the detection limits were 7.0-13.3ng/L; the average recoveries and relative standard deviations were 92.6%-94.5% and 0.9%-1.8%, respectively. For BPA, the methodology exhibited good linearity between 0.01 to 10 mg/L; the detection limit obtained by this method was 0.03μg/L; the recoveries of simulated seawater for 1.0 and 10.0μg/L were 86.5% and 83.1% with the relative standard deviations below 6%. In the last chapter, the method using salting out phase separation microextraction and HPLC was applied again for the determination of carbamate insecticides residues from water. Extraction solvent was iso-butyl alcohol and salting out agent was ammonium sulfate. A C18 column was used for separation with detection wavelength at 220nm; the mobile phase was a mixture of methanol and water (the ratio of volume was 53: 47). The detection limits were 0.4-5.7μg/L. The average recovery of pesticides ranged from 78.6% to 89.8% with the relative standard deviations below 5.0%.
引文
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