串联质谱法分析血浆中DHA和水中多氯联苯

发布时间：2018-01-17 02:29

本文关键词：串联质谱法分析血浆中DHA和水中多氯联苯　出处：《大连理工大学》2014年硕士论文　论文类型：学位论文

【摘要】：近年来,LC-MS、GC-MS技术逐渐成为常规分析仪器,但随着样品基质越来越复杂,待测物质种类越来越多,未知物质的鉴定需求也在增长,色质联用系统在很多情况下已经无法满足检测需求。而串联质谱由于更好的除干扰、更高的灵敏度和定量分析能力,成为质谱发展中的一大热点,在药物代谢、蛋白组学研究、食品安全、环境监测等领域得到广泛应用。本文采用串联质谱法分析了血浆中的二十二碳六烯酸(DHA)和水中的多氯联苯(PCBs)。对于DHA的分析,首先,以2-氨基-2-甲基-1-丙醇(AMP),作为血浆中DHA的杂环衍生试剂,优化了反应条件,建立了气相色谱-串联质谱(GC-MS/MS)分析方法。经过方法学研究,在0.07～10.00μg/mL的范围内,线性较好r2=0.9991；定量限是0.07μg/mL,最小检出限是0.02μg/ML;平均回收率为96.00%～104.16%。并对20组人血浆样品进行了分析,DHA浓度在1.532～2.524μg/g之间。其次,是采用C18固相萃取(SPE)小柱富集净化,建立了高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。经过方法学研究,在0.10～60.00μg/mL范围内,线性良好r2=0.9990；定量限是0.10μg/mL,最小检出限是0.04μg/mL;平均回收率为94.79%～101.09%。并对20组大鼠血浆进行了分析,DHA浓度在1.13～2.07μg/mL之间。两种方法均适于血浆中DHA的分析。对于PCBs的分析,本文采用分散液液微萃取(DLLME)法富集水中10种PCBs,对DLLME的五个因素采取了正交试验研究,确定了最佳萃取条件,建立了气相色谱-串联质谱(GC-MS/MS)分析方法。经过方法学研究,10种PCBs在2.5～1000.0ng/L范围内有良好线性r20.9990；检出限范围为0.1～0.5ng/L,定量限范围为0.4～2.5ng/L；三个添加水平下,平均回收率范围分别为91.60%～108.03%、95.40%～109.08%、90.43%～105.52%。采用该法对不同来源水进行了分析,只有环境水样检出了少量PCBs,矿泉水和自来水均未检出。
[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.

【学位授予单位】：大连理工大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：O657.63;R927.2

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