固相萃
發(fā)布時間:2018-05-23 22:15
本文選題:環(huán)境化學(xué)污染物 + 尿。 參考:《中國疾病預(yù)防控制中心》2017年碩士論文
【摘要】:環(huán)境化學(xué)污染物廣泛存在于人類生活環(huán)境中,可通過呼吸道、消化道和皮膚等進入人體內(nèi)產(chǎn)生多種健康危害效應(yīng),如呼吸系統(tǒng)、消化系統(tǒng)疾病,干擾內(nèi)分泌系統(tǒng)導(dǎo)致生殖發(fā)育系統(tǒng)異常等。污染物進入人體后迅速被吸收并經(jīng)肝腎等器官發(fā)生代謝,痕量化學(xué)污染物在樣品中含量很低,分布很不均勻,往往隨時間、空間變化波動很大,部分缺乏標(biāo)準(zhǔn)物質(zhì)測定困難,且空白干擾較大,如鄰苯二甲酸酯類在生物樣品中的檢測易受空白干擾,且不易去除。而對其在人體中的代謝物檢測不僅能有效避免空白干擾的問題,而且也能更準(zhǔn)確的反映在體內(nèi)的真實水平。尿液相對于其他生物基質(zhì),由于其對人體無損傷和取樣方便的特點備受國內(nèi)外學(xué)者的廣泛使用,是人群生物監(jiān)測常用的生物樣品。本研究采用固相萃取-超高效液相色譜-串聯(lián)質(zhì)譜技術(shù)建立同時測定人尿中鄰苯二甲酸酯類代謝物、多環(huán)芳烴類代謝物和雙酚A類化合物的分析方法,并對吸煙人群和非吸煙人群的尿樣進行了檢測。本論文得到的主要結(jié)論如下:目的:建立人尿中多種環(huán)境化學(xué)污染物代謝物的SPE-UPLC-MS/MS分析方法。方法:10 mL尿樣經(jīng)β-葡糖甘酸酶和硫酸酯酶水解過夜,水解液通過Bond Elut C18(500 mg/3 mL)固相萃取柱富集,2 mL乙酸乙酯緩慢洗脫后,氮氣吹至0.5 mL以下,再用3 mL乙腈緩慢洗脫后,30℃氮氣吹至0.5 mL上機分析。待測液經(jīng)Waters ACQUITYUPLC BEH C18 色譜柱(2.1 mm×100 mm,1.7 μm)分離,負(fù)電離模式(ESI-)、多反應(yīng)監(jiān)測(MRM)條件下分析,同位素內(nèi)標(biāo)法定量,測定人尿中10種PAEs代謝物、7種OH-PAHs和2種BPAs的含量。結(jié)果:該方法對尿中19種目標(biāo)化合物在0.078 ng/mL~40 ng/mL的線性范圍呈良好的線性關(guān)系,相關(guān)系數(shù)均大于0.9985。19種目標(biāo)化合物的檢出限(S/N=3)在0.02 ng/mL~0.41 ng/mL之間,定量限(S/N=10)在0.05ng/mL~1.36ng/mL之間。樣品在低、中、高三個濃度水平的平均加標(biāo)回收率為89.4%~114%,批內(nèi)精密度15%(MEHHP為15.8%,6-CHRY 為 22.2%),批間精密度15%(MEHP 為 17.1%,3-BAA 為 18.1%)。結(jié)論:本方法建立了同時測定人尿中19種環(huán)境化學(xué)污染物代謝物的固相萃取-超高效液相色譜-串聯(lián)質(zhì)譜分析方法。方法準(zhǔn)確度好,精密度高,適合人群生物監(jiān)測中多種生物標(biāo)志物含量同時測定。
[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,
本文編號:1926587
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