反向高效液相色譜法檢測污泥中含硫氨基酸
發(fā)布時間:2018-06-22 22:15
本文選題:含硫氨基酸 + 半胱氨酸。 參考:《中國環(huán)境科學(xué)》2017年12期
【摘要】:含硫氨基酸是污水廠污泥厭氧消化過程惡臭氣體H2S和VOSCS的主要前體物質(zhì),以污水廠濃縮污泥為研究對象,針對污泥成分復(fù)雜,其含硫蛋白難水解、難提純和易氧化而導(dǎo)致的尚無法定量檢測分析的難點(diǎn),通過優(yōu)化預(yù)處理?xiàng)l件、色譜條件參數(shù)等,建立了一種污泥中含硫氨基酸反相高效液相檢測的新方法.主要步驟為:50mg冷干污泥經(jīng)1.5mL過甲酸氧化30min,將其中的半胱氨酸和蛋氨酸氧化為磺基丙氨酸和蛋氨酸砜,于水解管進(jìn)行酸水解,3k D Millipore超濾離心,采用鄰苯二甲醛進(jìn)行柱前衍生,經(jīng)氨基柱分離,通過FLD檢測器檢測.測定結(jié)果表明,磺基丙氨酸和蛋氨酸砜的定量限分別為0.24和1.21μmol/L,并且在5~500μmol/L范圍內(nèi)均具有良好線性關(guān)系(R~2≥0.9997),加標(biāo)回收率均在90%以上.采用該方法測定污泥中的含硫氨基酸結(jié)果表明:濃縮污泥半胱氨酸和蛋氨酸含量分別為3.86和6.20mg/(g DS),160℃熱水解后,二者含量分別降低了48.0%和51.9%,且厭氧消化后兩種條件下含硫氨基酸的含量存在明顯差異,為探究厭氧消化體系下污泥中硫的代謝途徑和轉(zhuǎn)化機(jī)制提供了方法支撐.
[Abstract]:Sulfur-containing amino acids are the main precursors of malodorous gases H _ 2S and VOSCS in the anaerobic digestion process of sewage sludge. The concentrated sludge of wastewater treatment plant is taken as the research object. In view of the complex composition of sludge, the sulfur-containing protein is difficult to hydrolyze. It is difficult to detect and analyze quantitatively due to the difficulty of purification and easy oxidation. By optimizing the pretreatment conditions and chromatographic parameters, a new method for the determination of sulfur-containing amino acids in sludge by reversed-phase high performance liquid chromatography (RP-HPLC) has been established. The main steps were as follows: 1: 50mg cold dry sludge was oxidized by 1.5 mL performic acid for 30 min, the cysteine and methionine were oxidized to sulfoalanine and methionine sulfone for 30 min. The hydrolysate was centrifuged by 3kD Millipore ultrafiltration in the hydrolysate tube, and the precolumn derivatization was carried out by phthalaldehyde. It was separated by amino column and detected by FLD detector. The results showed that the quantification limits of sulfoalanine and methionine sulfone were 0.24 and 1.21 渭 mol / L, respectively, and the linear relationship was obtained in the range of 5 ~ 500 渭 mol / L (R ~ (2) 鈮,
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