水环境中磺胺类抗生素固相萃取-液质联用检测方法的建立及效果评估

为快速、同步检测分析磺胺类抗生素，有效削减并控制水体中磺胺类上抗生素含量，基于已有检测仪器和分析测试方法，建立了一种用于同时测定水体中8种磺胺类抗生素(磺胺氯哒嗪、磺胺间二甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲恶唑、磺胺喹恶啉、磺胺甲氧哒嗪、磺胺甲噻二唑、磺胺吡啶)残留的固相萃取-液相色谱-三重四极杆串联质谱检测方法；在检测过程中，调节水样的pH为3，用HLB固相萃取柱进行净化、富集，在40 ℃条件下用氮吹浓缩吹干，用超纯水复溶至1 mL；以0.1%甲酸水溶液和0.1%甲酸乙腈溶液作为流动相，使用Phenomenex Kinetex F5 色谱柱(50 mm×3.0 mm, 2.6 μm)进行分离，在多反应监测模式(MRM)下对样品进行定量、定性分析。结果表明：8种磺胺类抗生素线性关系良好，且拟合度均大于0.999 0；检出限为0.1~0.5 μg·L⁻¹，定量限为0.5~2.0 μg·L⁻¹；质量浓度为1、5、50 μg·L⁻¹的混标溶液的加标回收率分别为78.85%~127.96%、76.69%~114.38%和73.55%~125.92%, 相对标准偏差均在15%以内。该方法快捷、高效、灵敏，能够满足水中磺胺类抗生素的定性、定量检测，可为我国检测方法标准体系的建设提供参考。

Establishment of solid phase extraction-liquid mass spectrometry method for detection of sulfa antibiotics in water environment and its effect evaluation

In order to quickly and synchronously detect and analyze sulphonamides, effectively reduce and control sulphonamides content in water, based on the existing detection instruments and analysis and testing methods, a liquid chromatography-triple quadrupole tandem mass spectrometry method was developed to simultaneously detect the residues of 8 antibiotics in water: sulfadiazine, sulfadimethyrimidine, sulfadimethyrimidine, sulfamethoxazole, sulfamequinoline, sulfamethoxyazine, sulfamethothiazole, sulfamepyridine. During the detecting process, the sulfonamides in water samples were enriched with HLB solid phase extraction column at pH=3, then dried by nitrogen blowing at 40 ℃ and re-dissolved to 1mL by ultrapure water, lastly separated by Phenomenex Kinetex F5 column (50 mm×3.0 mm, 2.6 μm) using 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile as mobile phase. The results showed that there was a good linear relationship between the 8 sulfonamides antibiotics and the fitting degree was higher than 0.999. The limits of detection were 0.1~0.5 μg·L−1, and the limits of quantification were 0.5~2.0 μg·L−1. The recoveries of mixed standard solutions with mass concentrations of 1, 5 and 50 μg·L−1 were 78.85%~127.96%, 76.69%~114.38% and 73.55%~125.92%, respectively, and the relative standard deviations (RSD) were not higher than 15%. The method is quick, efficient and sensitive, and can satisfy the qualitative and quantitative detection of sulfa antibiotics in water. It can provide a reference for the construction of standard system of detection methods in China.