反向高效液相色谱法检测污泥中含硫氨基酸

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Abstract Sulfur-containing amino acids are the main precursor of H₂S and VOSC_S in sludge anaerobic digestion process. As the sulfur-containing protein in sewage sludge is difficult to be hydrolyzed, difficult to be extracted and easy to be oxidized, thus it is difficult to be quantified. Based on the optimal parameters of oxidation conditions, chromatographic conditions and etc., a quantitative analysis method of sulfur-containing amino acids in sewage sludge was established by reverse-phase high performance liquid chromatography coupled with pre-column derivatization. The main procedures are as following:Firstly, the cysteine and methionine in sludge (50mg) were respectively oxidized to cysteic acid and methionine sulfone by performic acid (1.5mL, 30min). Then, after ultrafiltration and derivatization by OPA, they were sequentially separated by NH₂ column and finally detected by FLD detector. A good linear relationship (corresponding linear correlation coefficient (R²) greater than 0.9997) was obtained with the high recoveries of cysteine and methionine (above 90%). In addition, the quantitation limits of cysteine and methionine were 0.24 and 0.12μmol/L respectively. The sulfur-containing amino acids in different sludge samples were quantified by using this method. In raw sludge, the cysteine and methionine contents were 3.86 and 6.20mg/(g DS) respectively, and decreased by 48.0% and 51.9% respectively after pyrohydrolysis treatment at 160℃. Moreover, a significant difference of sulfur-containing amino acids content between pyrohydrolysis treatment and non-pyrohydrolysis treatment can be found, which suggest that the generation and utilization mechanisms of sulfur-containing amino acids were different in different anaerobic digesters. However, the established method of this study can provide an effective support to study the metabolic pathways and transfer mechanism in digestion systems.

Key words： sulfur amino acids cysteine methionine sludge RP-HPLC

Received: 31 May 2017

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	XIONG Nan-an
	DONG Bin
	DAI Xiao-hu

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XIONG Nan-an,DONG Bin,DAI Xiao-hu. Determination of sulfur amino acids in sludge by RP-HPLC[J]. CHINA ENVIRONMENTAL SCIENCECE, 2017, 37(12): 4614-4619.

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http://www.zghjkx.com.cn/EN/ OR http://www.zghjkx.com.cn/EN/Y2017/V37/I12/4614

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