SPE-UFLC-MS法测定医药废水中8种四环素类抗生素

Determination of eight tetracyline antibiotics in phormaceutical wastewater by SPE-UFLC-MS method

建立了固相萃取-超高速液相色谱质谱(SPE-UFLC-MS)法测定医药废水中8种四环素类抗生素的方法。通过固相萃取条件优化,选择固相Oasis HLB萃取柱、净化剂为30%ZnSO_(4)+20%K_(2)[Fe(CN)_(4)]溶液、稳定剂为1g·L^(-1)的Na_(2)EDTA、萃取pH值为8,获得最佳目标化合物萃取回收率。8种四环素类抗生素的标准曲线线性关系良好(r>0.999),且检出限低于10ng·L^(-1),平均回收率为95.3%~106.9%,相对标准偏差RSD小于8.23%。方法精密度和准确度较好。经实样测试,医药废水的调质池中除地美环素盐酸盐和二甲胺四环素盐酸盐外,其他6种四环素类抗生素均有不同程度检出,可为医药废水抗生素类化合物检测提供借鉴。

A solid-phase extraction ultra high speed liquid chromatography-mass spectrometry(SPE-UFLC-MS)method was established for the determination of eight tetracycline antibiotics in pharmaceutical wastewater.By optimizing the conditions of solid-phase extraction,a solid-phase Oasis HLB extraction column,a purification agent of 30%zinc sulfate+20%potassium ferrocyanide solution,a stabilizer of 1g·L^(-1)Na_(2)EDTA,and an extraction pH value of 8 were selected to obtain the optimal extraction recovery rate of the target compound.The standard curves of eight tetracycline antibiotics have a good linear relationship(r>0.999)and the detection limit is less than 10ng·L^(-1).The average recovery rate is 95.3%~106.9%,and the relative standard deviation(RSD)is less than 8.23%.The method has good precision and accuracy.After actual sample testing,except for dexamethasone hydrochloride and dimethylamine tetracycline hydrochloride,the other 6 tetracycline antibiotics were detected to varying degrees in the conditioning tank of pharmaceutical wastewater.This can provide reference for the detection of antibiotic compounds in pharmaceutical wastewater.