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目的建立固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)分析方法同时测定5个污水处理厂进出水中7类14种抗生素的残留量。方法水样经过滤后,添加适量乙二胺四乙酸二钠(100 mg·L~(-1))并用盐酸调节p H值为4.0。采用Cleanert PEP-2固相萃取柱对水样中的目标化合物进行富集、净化。采用Waters ACQUITY UPLC~BEH Phenyl(50 mm×2.1 mm,1.7μm)色谱柱,流动相为乙腈和体积分数0.1%的甲酸水溶液。质谱检测采用ESI源正负离子同时扫描,多反应检测模式(MRM)。结果目标分析物在各自的线性范围内峰面积与质量浓度线性关系良好,r为0.998 1~0.999 9。方法检测限为0.04~3.89 ng·L~(-1)。14种抗生素的加标平均回收率为46.68%~98.31%,RSD为2.39%~11.05%(n=9)。使用标准添加法定量以减小基质效应的影响。用此法对5个污水处理厂进出水中14种抗生素进行定量检测,大多数抗生素能检出,表明污水处理厂的处理工艺并没有完全去除抗生素,大多数抗生素又2次排入水体。结论该方法适用于污水中抗生素类药物的检测。
OBJECTIVE To establish a solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS / MS) method for the simultaneous determination of 7 classes of 14 antibiotics in the effluent of five WWTPs. Method After the water sample was filtered, add appropriate amount of ethylenediaminetetraacetic acid (100 mg · L -1) and adjust the pH value to 4.0 with hydrochloric acid. The target compound in water sample was enriched and purified by using Cleanert PEP-2 solid phase extraction column. A Waters ACQUITY UPLC ~ BEH Phenyl (50 mm × 2.1 mm, 1.7 μm) column was used. The mobile phase consisted of acetonitrile and 0.1% aqueous formic acid. MS detection using ESI source positive and negative ions simultaneous scanning, multiple reaction detection mode (MRM). Results There was a good linear relationship between the peak area and the mass concentration of target analytes in their respective linear ranges, with r ranging from 0.998 1 to 0.999 9. The detection limit was 0.04 ~ 3.89 ng · L -1. The average recoveries of 14 antibiotics were 46.68% ~ 98.31% with RSDs of 2.39% ~ 11.05% (n = 9). Quantification using standard addition methods to reduce the effects of matrix effects. Quantitative detection of 14 antibiotics entering and exiting the water from the 5 WWTPs by this method can detect most of the antibiotics, indicating that the treatment process of the WWTP does not completely remove the antibiotics and most of the antibiotics are discharged into the water twice. Conclusion The method is suitable for the detection of antibiotics in wastewater.