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生物檢材中百草枯提取凈化及檢測(cè)方法的研究

發(fā)布時(shí)間:2018-06-27 20:03

  本文選題:百草枯 + 生物檢材 ; 參考:《昆明醫(yī)學(xué)院》2005年碩士論文


【摘要】:[目的] 百草枯(英文名,paraquat)屬滅生性除草劑,極性較強(qiáng),極易溶于水,在實(shí)際檢案中提取液難于濃縮,這是百草枯中毒案件分析鑒定中的一個(gè)巨大障礙。本課題采用離子對(duì)固相萃取(SPE)法提取百草枯,解決了凈化及濃縮問(wèn)題,建立高效液相色譜(HPLC)的定性定量分析方法,同時(shí)建立了毛細(xì)管電泳(HPCE)的定性分析方法。并進(jìn)一步通過(guò)動(dòng)植物中毒實(shí)驗(yàn)來(lái)驗(yàn)證所建立的提取、分離及檢測(cè)方法的可行性和準(zhǔn)確性。[方法] 植物檢材直接進(jìn)行離子對(duì)固相萃取,生物檢材經(jīng)糜蛋白酶酶解后進(jìn)行萃取,用HPLC定性定量分析,同時(shí)用TLC和HPCE進(jìn)行定性分析。[結(jié)果] 生物檢材的回收率在81%~94%之間,標(biāo)準(zhǔn)偏差在2.98~3.95%之間,變異系數(shù)在3.6~4.4%,最低檢測(cè)限1ng·ml~(-1)。[結(jié)論] 離子對(duì)固相萃取法提取百草枯的選擇性強(qiáng),具有提取率高、提取物干凈、重現(xiàn)性好等優(yōu)點(diǎn),HPLC/DAD法定性定量結(jié)果準(zhǔn)確、靈敏、重現(xiàn)性好;TLC法簡(jiǎn)單、快速易于在基層推廣,HPCE法也可用于百草枯分析。本方法可用于其它各類檢材中百草枯的檢測(cè),應(yīng)用范圍較廣。本研究為百草枯農(nóng)藥致農(nóng)作物枯死案件或致人畜中毒案件的分析鑒定提供了理論依據(jù)和快速、準(zhǔn)確的檢測(cè)方法。方法具有創(chuàng)新性、實(shí)用性和很高的推廣應(yīng)用價(jià)值。
[Abstract]:[objective] Paraquat is a kind of herbicide with strong polarity and easily soluble in water. It is difficult to concentrate the extract of paraquat in practical cases, which is a great obstacle in the analysis and identification of paraquat poisoning cases. In this paper, ion-pair solid phase extraction (SPE) was used to extract paraquat, which solved the problem of purification and concentration. The qualitative and quantitative analysis method of high performance liquid chromatography (HPLC) and capillary electrophoresis (HPCE) were established. Furthermore, the feasibility and accuracy of the established methods for extraction, separation and detection were verified by animal and plant poisoning experiments. [methods] Plant samples were extracted directly by ion pair solid phase extraction, and biological samples were extracted by chymotrypsin enzymatic hydrolysis. Qualitative analysis was performed by HPLC and TLC and HPCE at the same time. [results] the recoveries of biological samples were between 81% and 94%, the standard deviation was between 2.98% and 3.95%, the coefficient of variation was 3.66%, and the lowest detection limit was 1ng ml ~ (-1). [conclusion] Ion-pair solid-phase extraction method has the advantages of high selectivity, high extraction rate, clean extract and good reproducibility. The qualitative and quantitative results of HPLC / dad method are accurate, sensitive and reproducible. HPCE method can also be used for paraquat analysis. This method can be used for the detection of paraquat in other kinds of materials. This study provides a theoretical basis and a rapid and accurate method for the analysis and identification of paraquat pesticide-induced crop death cases or human and animal poisoning cases. The method is innovative, practical and valuable in popularization and application.
【學(xué)位授予單位】:昆明醫(yī)學(xué)院
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2005
【分類號(hào)】:D919

【參考文獻(xiàn)】

相關(guān)期刊論文 前3條

1 王朝虹,李玉安,邢俊波,張繼宗,張春水;高效液相色譜法測(cè)定人血液中的百草枯[J];中國(guó)法醫(yī)學(xué)雜志;2004年03期

2 喬靜,楊士云,潘冠民;百草枯的HPLC分析[J];刑事技術(shù);2000年02期

3 羅曉芳,王翠,王國(guó)榮;分光光度法測(cè)定紅蝦中的百草枯[J];中國(guó)衛(wèi)生檢驗(yàn)雜志;2001年06期

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