發(fā)布時(shí)間：2018-04-29 16:20

  本文選題：磁固相萃取 + 液液萃取�。� 參考：《青島理工大學(xué)》2015年碩士論文

【摘要】：磺酰脲類除草劑在治理雜草方面使用甚廣。這類除草劑水溶性較強(qiáng),易造成水體污染,在土壤中殘留會(huì)對(duì)后茬較為敏感的農(nóng)作物造成極大危害,對(duì)皮膚、眼睛、粘膜等也有一定的刺激作用。由于這類物質(zhì)在環(huán)境水樣中含量很低,為提高檢測(cè)的靈敏度及準(zhǔn)確度,還需在檢測(cè)前進(jìn)行必要的樣品前處理操作。本論文選取在我國使用范圍較廣的一些磺酰脲類除草劑化合物為目標(biāo)分析物,建立測(cè)定其在環(huán)境水體中含量的分析方法。分別采用液液萃取(LLE)、固相柱萃取(SPE)及磁固相萃取(MSPE)作為樣品前處理方法,高效液相色譜(HPLC)-紫外檢測(cè)為分離檢測(cè)手段,進(jìn)行了系統(tǒng)的研究。主要內(nèi)容如下:(1)建立了環(huán)境水樣中10種磺酰脲類除草劑的LLE-HPLC分析方法。在確定的色譜分離條件下,優(yōu)化了萃取劑的種類與體積、萃取次數(shù)、萃取時(shí)間與靜置時(shí)間、水樣p H及鹽濃度。方法線性范圍在0.02~10.0mg/L之間,檢出限在0.017~0.063μg/L之間,可以滿足歐盟《用水法則》中規(guī)定的農(nóng)藥限值小于1-5μg/L的測(cè)定要求。對(duì)青島市棘洪灘水庫地表水進(jìn)行精密度與準(zhǔn)確度的考察,相對(duì)標(biāo)準(zhǔn)偏差(RSD)小于14.1%,加標(biāo)回收率在73.0%~104.6%之間。該方法無需復(fù)雜設(shè)備,操作簡(jiǎn)單,便于普及。(2)建立了環(huán)境水樣中10種磺酰脲類除草劑的SPE-HPLC分析方法。采用C18固相萃取柱,優(yōu)化了洗脫劑的種類與體積、水樣p H及鹽濃度等固相萃取條件。方法線性范圍在0.02~10.0mg/L之間,檢出限在0.014~0.032μg/L之間。對(duì)地表水進(jìn)行精密度與準(zhǔn)確度的考察,其相對(duì)標(biāo)準(zhǔn)偏差(RSD)小于13.0%,加標(biāo)回收率在75.6%~110.6%之間。該方法比液液萃取法所用洗脫溶劑少,可同時(shí)進(jìn)行多個(gè)水樣的操作。(3)建立了環(huán)境水樣中6種磺酰脲類除草劑的MSPE-HPLC分析方法。自制磁性多壁碳納米管,采用X-射線衍射對(duì)其表征�？疾炝擞绊懘判怨滔噍腿⌒实囊蛩�,諸如吸附劑用量、水樣p H、鹽濃度、萃取及解析時(shí)間、洗脫劑種類及用量等,確定了最佳萃取條件。線性范圍在0.02~10.0mg/L之間,檢出限在0.001μg/L~0.004μg/L之間。對(duì)地表水進(jìn)行精密度與準(zhǔn)確度的考察,其相對(duì)標(biāo)準(zhǔn)偏差(RSD)小于9.8%,加標(biāo)回收率在84.9%~106.9%之間;對(duì)自來水進(jìn)行精密度與準(zhǔn)確度的考察,其相對(duì)標(biāo)準(zhǔn)偏差(RSD)小于11.3%,加標(biāo)回收率在78.2%~105.4%之間。該方法無需復(fù)雜儀器,操作簡(jiǎn)單、省時(shí),具有較高的靈敏度。可應(yīng)用于環(huán)境水樣中磺酰脲類除草劑的檢測(cè)。
[Abstract]:Sulfonylurea herbicides are widely used in weed control. This kind of herbicide is water-soluble and easy to cause water pollution. Residues in the soil will cause great harm to the crops which are more sensitive to the next crop. It will also stimulate the skin, eyes, mucous membrane and so on. Due to the low content of these substances in environmental water samples, in order to improve the sensitivity and accuracy of detection, it is necessary to carry out the necessary sample pretreatment before detection. In this paper, some sulfonylurea herbicide compounds which are widely used in China are selected as target analytes, and a method for determination of their contents in environmental water is established. The methods of liquid-liquid extraction (LLE), solid phase column extraction (SPE) and magnetic solid phase extraction (MSPE) were used as sample pretreatment methods, and HPLCC-UV detection was used as the separation and detection method. The main contents are as follows: 1) A LLE-HPLC method for the determination of 10 sulfonylurea herbicides in environmental water samples was established. Under certain chromatographic separation conditions, the types and volume of extractant, extraction times, extraction time and static time, water sample pH and salt concentration were optimized. The linear range was between 0.02~10.0mg/L and the detection limit was 0.017 ~ 0.063 渭 g / L, which could meet the determination requirement of the pesticide limit of 1-5 渭 g / L. The precision and accuracy of surface water of Zhihongtan Reservoir in Qingdao City were investigated. The relative standard deviation (RSD) was less than 14.1and the recovery rate was between 73.0% and 104.6%. The method is simple and easy to operate without complicated equipment. It is easy to be popularized. The SPE-HPLC method for the determination of 10 sulfonylurea herbicides in environmental water samples has been established. C18 solid phase extraction column was used to optimize the conditions of solid phase extraction, such as the type and volume of eluent, water sample pH and salt concentration. The linear range was between 0.02~10.0mg/L and the detection limit was 0.014 渭 g / L. The relative standard deviation (RSDs) of surface water was less than 13.0 and the recovery rate was between 75.6% and 110.6%. This method has less elution solvent than liquid-liquid extraction method, and can be operated on several water samples at the same time. A MSPE-HPLC method for the determination of 6 sulfonylurea herbicides in environmental water samples was established. Magnetic multi-wall carbon nanotubes were prepared and characterized by X-ray diffraction. The factors affecting the efficiency of magnetic solid phase extraction (SPE), such as the amount of adsorbent, water sample pH, salt concentration, extraction and desorption time, the type and amount of eluant, etc., were investigated. The optimum extraction conditions were determined. The linear range is between 0.02~10.0mg/L and the detection limit is 0.001 渭 g/L~0.004 渭 g / L. The relative standard deviation (RSDs) of surface water was less than 9.8, and the recovery rate was between 84.9% and 106.9%. The relative standard deviation (RSDs) of surface water was less than 11.3and the recovery rate was between 78.2% and 105.4%. The method is simple, time saving and high sensitivity. It can be applied to the determination of sulfonylurea herbicides in environmental water samples.
【學(xué)位授予單位】：青島理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：X832

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本文編號(hào)：1820674