固相萃

发布时间：2018-05-23 22:15

  本文选题：环境化学污染物 + 尿　； 参考：《中国疾病预防控制中心》2017年硕士论文

【摘要】：环境化学污染物广泛存在于人类生活环境中,可通过呼吸道、消化道和皮肤等进入人体内产生多种健康危害效应,如呼吸系统、消化系统疾病,干扰内分泌系统导致生殖发育系统异常等。污染物进入人体后迅速被吸收并经肝肾等器官发生代谢,痕量化学污染物在样品中含量很低,分布很不均匀,往往随时间、空间变化波动很大,部分缺乏标准物质测定困难,且空白干扰较大,如邻苯二甲酸酯类在生物样品中的检测易受空白干扰,且不易去除。而对其在人体中的代谢物检测不仅能有效避免空白干扰的问题,而且也能更准确的反映在体内的真实水平。尿液相对于其他生物基质,由于其对人体无损伤和取样方便的特点备受国内外学者的广泛使用,是人群生物监测常用的生物样品。本研究采用固相萃取-超高效液相色谱-串联质谱技术建立同时测定人尿中邻苯二甲酸酯类代谢物、多环芳烃类代谢物和双酚A类化合物的分析方法,并对吸烟人群和非吸烟人群的尿样进行了检测。本论文得到的主要结论如下:目的:建立人尿中多种环境化学污染物代谢物的SPE-UPLC-MS/MS分析方法。方法:10 mL尿样经β-葡糖甘酸酶和硫酸酯酶水解过夜,水解液通过Bond Elut C18(500 mg/3 mL)固相萃取柱富集,2 mL乙酸乙酯缓慢洗脱后,氮气吹至0.5 mL以下,再用3 mL乙腈缓慢洗脱后,30℃氮气吹至0.5 mL上机分析。待测液经Waters ACQUITYUPLC BEH C18 色谱柱(2.1 mm×100 mm,1.7 μm)分离,负电离模式(ESI-)、多反应监测(MRM)条件下分析,同位素内标法定量,测定人尿中10种PAEs代谢物、7种OH-PAHs和2种BPAs的含量。结果:该方法对尿中19种目标化合物在0.078 ng/mL～40 ng/mL的线性范围呈良好的线性关系,相关系数均大于0.9985。19种目标化合物的检出限(S/N=3)在0.02 ng/mL～0.41 ng/mL之间,定量限(S/N=10)在0.05ng/mL～1.36ng/mL之间。样品在低、中、高三个浓度水平的平均加标回收率为89.4%～114%,批内精密度15%(MEHHP为15.8%,6-CHRY 为 22.2%),批间精密度15%(MEHP 为 17.1%,3-BAA 为 18.1%)。结论:本方法建立了同时测定人尿中19种环境化学污染物代谢物的固相萃取-超高效液相色谱-串联质谱分析方法。方法准确度好,精密度高,适合人群生物监测中多种生物标志物含量同时测定。
[Abstract]:Environmental chemical pollutants widely exist in human living environment. They can enter the human body through respiratory tract, digestive tract and skin, and produce many health hazard effects, such as respiratory system, digestive system diseases, etc. Endocrine disruptions lead to abnormal reproductive and developmental systems. After entering the human body, pollutants are quickly absorbed and metabolized by organs such as liver and kidney. Trace chemical pollutants in the samples are very low in content and uneven in distribution, and often fluctuate greatly with time and space, so it is difficult to determine some of them without reference materials. For example, the detection of phthalates in biological samples is easily affected by blank interference and is difficult to remove. The detection of metabolites in human body can not only effectively avoid the problem of blank interference, but also more accurately reflect the real level in the body. Compared with other biological substrates, urine is widely used by scholars at home and abroad because of its characteristics of no damage to human body and convenient sampling. Urine is a commonly used biological sample for human biological monitoring. A method for simultaneous determination of phthalate metabolites, polycyclic aromatic hydrocarbons (PAHs) and bisphenol A compounds in human urine by solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry was developed. Urine samples of smokers and non-smokers were tested. The main conclusions obtained in this paper are as follows: objective: to establish a SPE-UPLC-MS/MS method for the determination of metabolites of environmental chemical pollutants in human urine. Methods urine samples of 10 mL of urine were hydrolyzed overnight by 尾 -glucosaminidase and sulfate enzyme. The hydrolysate was enriched by Bond Elut C186500 mg/3 mL solid phase extraction column. After slowly eluting 2 mL ethyl acetate, nitrogen was blown below 0.5 mL. After slowly eluting with 3 mL acetonitrile, nitrogen was blown to 0.5 mL at 30 鈩，

本文编号：1926587