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目的建立专属、灵敏的固相萃取-液相色谱分析方法测定污水处理厂出水中6种残留药物(氯霉素、青霉素、水杨酸、泼尼松、尼莫地平、辛伐他汀)的质量浓度。方法样品经PEP固相萃取小柱预处理后,用HPLC法测定。色谱柱:C18柱(200 mm×4.6 mm,5μm);流动相:甲醇-体积分数0.2%乙酸水溶液,梯度洗脱;流速:1.0 mL.min-1;检测波长:230 nm。结果氯霉素、青霉素、水杨酸、泼尼松、尼莫地平、辛伐他汀质量浓度分别在0.2～20.0 mg.L-1、1.0～100.0 mg.L-1、0.1～10.0 mg.L-1、0.2～20.0 mg.L-1、0.1～10.0 mg.L-1、0.1～10.0 mg.L-1内线性关系良好,相关系数均大于0.999 3,精密度(RSD)为1.1%～1.9%,平均加样回收率在73.1%～100.2%内,样品溶液在12 h内稳定性良好。结论该方法简单、灵敏、准确,可用于水环境中残留药物的分析。
Objective To establish an accurate and sensitive method for the determination of six residual drugs (chloramphenicol, penicillin, salicylic acid, prednisone, nimodipine and simvastatin) in effluent of sewage treatment plants by liquid chromatography concentration. Methods The samples were pretreated with PEP solid phase extraction cartridges and determined by HPLC method. Column: C18 column (200 mm × 4.6 mm, 5 μm); mobile phase: methanol-water 0.2% acetic acid aqueous solution, gradient elution; flow rate: 1.0 mL.min-1; detection wavelength: 230 nm. Results The concentrations of chloramphenicol, penicillin, salicylic acid, prednisone, nimodipine and simvastatin were 0.2 ~ 20.0 mg.L-1, 1.0 ~ 100.0 mg.L-1, 0.1 ~ 10.0 mg.L -1,0.2 ~ 20.0 mg.L-1, 0.1 ~ 10.0 mg.L-1, 0.1 ~ 10.0 mg.L-1, the correlation coefficients were all greater than 0.999 3, the RSD was 1.1% 1.9%, the average recovery was within 73.1% ~ 100.2%. The stability of the sample solution was good within 12 h. Conclusion The method is simple, sensitive and accurate and can be used for the analysis of residual drug in water environment.