高效液相色谱串联质谱法测定污水污泥中4种磺胺类药物及其乙酰化代谢物

Determination of four sulfonamides and their corresponding acetyl metabolites in wastewater and sludge by high performance liquid chromatography tandem mass spectrometry

本文建立了一种检测污水及污泥中4种磺胺类抗生素及其相应的乙酰化代谢物的分析方法,包括磺胺嘧啶(SD)、磺胺甲基嘧啶(SM1)、磺胺二甲基嘧啶(SM2)、磺胺甲恶唑(SMZ)以及它们相对应的乙酰化代谢物.本文采用了固相萃取(SPE)的方法作为前处理,并优化了固相萃取条件.计算了样品中复杂的基质效应,并使用内标法来抵消基质效应.该方法在污水中检测限(LOD)和定量限(LOQ)分别为0.12—2.06 ng·L^(-1)和0.43—5.12 ng·L^(-1),在污泥中分别为0.28—2.31 ng·g^(-1)和0.88—6.77 ng·g^(-1),在污水和污泥中的回收率为分别为70.8%—130.6%,88.0%—129.2%.本方法成功应用于检测污水处理厂中的污水及污泥中的目标化合物.

An analytical method for the simultaneous determination of four sulfonamides and their corresponding acetyl metabolites was developed. The target analytes were sulfadiazine（SD）,sulfamerazine（SM1）,sulfamethazine（SM2）,sulfamethoxazole（ SMZ） and their acetyl metabolites.Solid phase extraction（SPE） was used for the purification and the SPE conditions were optimized.Matrix effects were evaluated and compensated using internal standard. The limits of detection（ LOD） and limits of quantification（ LOQ） were 0.12—2.06 ng·L^（-1） and 0. 43—5. 12 ng·L^（-1） for wastewater and 0.28—2.31 ng·L^（-1）and 0.88—6.77 ng·L^（-1） for sludge,respectively. Recoveries of the target compounds ranged from 70.8% to 130.6% in wastewater and 88.0% to 129.2% in sludge. The method was successfully applied to analyze target compounds in wastewater and sludge samples in wastewater treatment plants（ WWTPs）.