水和土壤中磺胺和激素类药物的同时分析方法

    Method for Simultaneous Determination of Sulfonamides and Hormone-Type Drugs in Water and Soil

    • 摘要: 建立了一种水和土壤中磺胺嘧啶、磺胺甲嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺二甲氧嘧啶、磺胺甲恶唑6种磺胺类药物和17α-雌二醇、17β-雌二醇、雌酮、雌三醇、炔雌醇、乙烷雌酚6种激素类药物同时分析的方法。具体步骤:水样过滤后使用Oasis HLB 固相萃取小柱进行净化富集;土壤样品经加速溶剂提取(ASE)之后过Oasis HLB小柱净化富集;采用超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测,分别以乙腈和1 mL•L-1甲酸溶液、乙腈和1 mL•L-1氨水溶液作为流动相。磺胺在水和土壤中的回收率分别为87.4%~103.6%和58.2%~80.0%,激素在水和土壤中的回收率分别为84.8%~101.8%和62.8%~79.3%,相对标准偏差均小于10.3%。水和土壤中磺胺的检测限分别为0.11~0.24 ng•L-1和0.01~0.02 ng•g-1,激素的检测限分别为0.31~2.14 ng•L-1和0.03~0.21 ng•g-1。用上述方法检测宿迁某典型养殖场周边的地表水和土壤,结果表明采用该方法检测环境样品中的磺胺和激素类药物是可行的。

       

      Abstract: A new method has been established for simultaneous determination of 6 sulfonamides, i.e. sulfadiazine, sulfamerazine, sulfathiazole, sulfamethazine, sulfadimethazine, sulfamethoxazole, and 6 hormone-type drugs, i.e. 17α-estradiol, 17β-estradiol, estrone, estriol, 17α-ethinyl-estradiol and hexestrol. Specific steps of the method are as following: After being filtered, water samples get purified and concentrated through Oasis HLB solid-phase extraction (SPE) cartridges. After accelerated solvent extraction (ASE), soil samples get purified and concentrated through Oasis HLB cartridges. Then the water and soil samples are analyzed by UPLC-MS/MS, which uses solvent of acetonitrile-and-methanoic acid (1 mL•L-1) and acetonitrile-and-ammonia (1 mL•L-1) as mobile phase respectively. The mean recovery rate of sulfonamides in water and soil samples varied in the range of 87.4-103.6% and 58.2-80.0%, respectively, and that of the hormones in the range of 84.8%-101.8% and 62.8%-79.3%, respectively, with relative standard deviation all below 10.3%. Detection limit of the method (MDL) for sulfonamides in water and soil ranged from 0.11 to 0.24ng•L-1 and from 0.01 to 0.02ng.g-1, respectively, and for the hormones did from 0.31 to 2.14 ng•L-1 and from 0.03 to 0.21 ng•L-1, respectively. This method was applied for determination of sulfonamides and hormones in the soil and surface water around a swine farm typical in Suqian area, with results demonstrating that this method is applicable to the determination of sulfonamides and hormone-type drugs in the environment.

       

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