反向高效液相色谱法检测污泥中含硫氨基酸

发布时间：2018-06-22 22:15

  本文选题：含硫氨基酸 + 半胱氨酸　； 参考：《中国环境科学》2017年12期

【摘要】：含硫氨基酸是污水厂污泥厌氧消化过程恶臭气体H2S和VOSCS的主要前体物质,以污水厂浓缩污泥为研究对象,针对污泥成分复杂,其含硫蛋白难水解、难提纯和易氧化而导致的尚无法定量检测分析的难点,通过优化预处理条件、色谱条件参数等,建立了一种污泥中含硫氨基酸反相高效液相检测的新方法.主要步骤为:50mg冷干污泥经1.5mL过甲酸氧化30min,将其中的半胱氨酸和蛋氨酸氧化为磺基丙氨酸和蛋氨酸砜,于水解管进行酸水解,3k D Millipore超滤离心,采用邻苯二甲醛进行柱前衍生,经氨基柱分离,通过FLD检测器检测.测定结果表明,磺基丙氨酸和蛋氨酸砜的定量限分别为0.24和1.21μmol/L,并且在5~500μmol/L范围内均具有良好线性关系(R~2≥0.9997),加标回收率均在90%以上.采用该方法测定污泥中的含硫氨基酸结果表明:浓缩污泥半胱氨酸和蛋氨酸含量分别为3.86和6.20mg/(g DS),160℃热水解后,二者含量分别降低了48.0%和51.9%,且厌氧消化后两种条件下含硫氨基酸的含量存在明显差异,为探究厌氧消化体系下污泥中硫的代谢途径和转化机制提供了方法支撑.
[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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