本文關(guān)鍵詞：串聯(lián)質(zhì)譜法分析血漿中DHA和水中多氯聯(lián)苯　出處：《大連理工大學(xué)》2014年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 二十二碳六烯酸(DHA) 雜環(huán)衍生化 固相萃取(SPE) 多氯聯(lián)苯(PCBs) 分散液液微萃取(DLLME)

【摘要】：近年來,LC-MS、GC-MS技術(shù)逐漸成為常規(guī)分析儀器,但隨著樣品基質(zhì)越來越復(fù)雜,待測物質(zhì)種類越來越多,未知物質(zhì)的鑒定需求也在增長,色質(zhì)聯(lián)用系統(tǒng)在很多情況下已經(jīng)無法滿足檢測需求。而串聯(lián)質(zhì)譜由于更好的除干擾、更高的靈敏度和定量分析能力,成為質(zhì)譜發(fā)展中的一大熱點,在藥物代謝、蛋白組學(xué)研究、食品安全、環(huán)境監(jiān)測等領(lǐng)域得到廣泛應(yīng)用。本文采用串聯(lián)質(zhì)譜法分析了血漿中的二十二碳六烯酸(DHA)和水中的多氯聯(lián)苯(PCBs)。 對于DHA的分析,首先,以2-氨基-2-甲基-1-丙醇(AMP),作為血漿中DHA的雜環(huán)衍生試劑,優(yōu)化了反應(yīng)條件,建立了氣相色譜-串聯(lián)質(zhì)譜(GC-MS/MS)分析方法。經(jīng)過方法學(xué)研究,在0.07～10.00μg/mL的范圍內(nèi),線性較好r2=0.9991；定量限是0.07μg/mL,最小檢出限是0.02μg/ML;平均回收率為96.00%～104.16%。并對20組人血漿樣品進行了分析,DHA濃度在1.532～2.524μg/g之間。其次,是采用C18固相萃取(SPE)小柱富集凈化,建立了高效液相色譜-串聯(lián)質(zhì)譜(HPLC-MS/MS)分析方法。經(jīng)過方法學(xué)研究,在0.10～60.00μg/mL范圍內(nèi),線性良好r2=0.9990；定量限是0.10μg/mL,最小檢出限是0.04μg/mL;平均回收率為94.79%～101.09%。并對20組大鼠血漿進行了分析,DHA濃度在1.13～2.07μg/mL之間。兩種方法均適于血漿中DHA的分析。 對于PCBs的分析,本文采用分散液液微萃取(DLLME)法富集水中10種PCBs,對DLLME的五個因素采取了正交試驗研究,確定了最佳萃取條件,建立了氣相色譜-串聯(lián)質(zhì)譜(GC-MS/MS)分析方法。經(jīng)過方法學(xué)研究,10種PCBs在2.5～1000.0ng/L范圍內(nèi)有良好線性r20.9990；檢出限范圍為0.1～0.5ng/L,定量限范圍為0.4～2.5ng/L；三個添加水平下,平均回收率范圍分別為91.60%～108.03%、95.40%～109.08%、90.43%～105.52%。采用該法對不同來源水進行了分析,只有環(huán)境水樣檢出了少量PCBs,礦泉水和自來水均未檢出。
[Abstract]:In recent years, LC-MS, GC-MS technology has gradually become a routine analytical instrument, but with the sample matrix is more and more complex, more and more types of material to be measured, identification of unknown material demand is also increasing in the system, in many cases have been unable to meet the needs of detection of GC-MS and tandem mass spectrometry. In addition due to the interference of better sensitivity and ability. Quantitative analysis of higher, become a hot topic in the development of mass spectrometry, in drug metabolism studies, protein food safety, is widely used in the field of environmental monitoring. In this paper, by using tandem mass spectrometry analysis in the plasma of twenty-two carbon six acid (DHA) and polychlorinated biphenyls (PCBs) in water.
For DHA analysis, first of all, with 2- amino -2- methyl -1- propanol (AMP), plasma DHA heterocycles as derivatization reagent, the reaction conditions were optimized, the establishment of a gas chromatography tandem mass spectrometry (GC-MS/MS) analysis method. Through the study, in 0.07 ~ 10 g/mL range, good linearity of r2=0.9991; quantitation limit is 0.07 g/mL, the minimum detection limit is 0.02 g/ML; the average recovery rate was 96% ~ 104.16%. and 20 groups of human plasma samples were analyzed, the DHA concentration between 1.532 ~ 2.524 g/g. Secondly, using C18 solid phase extraction (SPE) were enriched and purified, HPLC tandem mass spectrometry (HPLC-MS/MS) analysis method. Through the study, in 0.10 ~ 60 g/mL range, a good linear r2=0.9990; the quantitation limit is 0.10 g/mL, the minimum detection limit is 0.04 g/mL; the average recovery rate was 94.79% ~ 101.09%. and plasma of 20 groups of rats were analyzed, The concentration of DHA is between 1.13 and 2.07 mu g/mL. The two methods are suitable for the analysis of DHA in plasma.
For PCBs analysis, this paper using dispersive liquid-liquid microextraction (DLLME) enrichment of water of 10 PCBs, the five factors of DLLME adopted the orthogonal experiments, the optimum condition was confirmed, a gas chromatography tandem mass spectrometry (GC-MS/MS) analysis method. Through the research methodology, 10 in PCBs the range of 2.5 ~ 1000.0ng/L has a good linear r20.9990; the detection limit range is 0.1 ~ 0.5ng/L, the quantitative limit is 0.4 ~ 2.5ng/L; three levels, the average recovery rate ranges were 91.60% ~ 108.03%, 95.40% ~ 109.08%, 90.43% ~ 105.52%. by the method of different sources of water are analyzed, only water detection a small amount of PCBs, mineral water and tap water were not detected.

【學(xué)位授予單位】：大連理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2014
【分類號】：O657.63;R927.2

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