固相萃取-高效液相色谱法测定地表水中4种磺胺类抗生素

摘要

建立固相萃取-高效液相色谱法测定地表水中磺胺嘧啶、磺胺二甲嘧啶、磺胺氯哒嗪、醋磺胺甲恶唑4种磺胺类抗生素.样品采用HLB柱进行萃取富集,流动相为甲醇-水(体积比为20:80),流量为0.5 mL/min,用SPD检测器检测,检测波长为270 nm;采用外标法定量.4种磺胺类抗生素质量浓度在4~160 ng/L范围内与色谱峰面积的线性关系良好,相关系数不低于0.9982,方法检出限为1.0~1.7 ng/L,样品加标回收率为75.2%~97.4%,测定结果的相对标准偏差为2.8%~6.1%(n=7).该方法操作简便,灵敏度高,可用于地表水中磺胺类抗生素的检测.%A method was established for determining sulfadiazine, sulfadimidine, sulfachloropyridazine, acetylsulfamethoxazole in surface water by high performance liquid chromatography with solid phase extraction. The sample was extracted and enriched by Oasis HLB column. The mobile phase was methanol-water(volum rate was 20:80) with flow rate of 0.5 mL/min.The sample was detected by SPD detector on detecting wavelengths of 270 nm. External standard method was used for quantitative analysis. The mass concentration of four sulfonamide antibiotics showed good linear relationships with the chromatography peak area in the range of 4-160 ng/L, the correlation coefficients were not less than 0.998 2. The method detection limits were 1.0-1.7 ng/L. The average recoveries for four sulfonamide antibiotics were 75.2%-97.4%, the relative standard deviations of determinition results were 2.8%-6.1%(n=7). The method is simple and sensitive, which can be applied to the analysis of sulfonamide antibiotics in surface water.