建立了同时检测河流底泥中12种抗生素(4种磺胺类、3种喹诺酮类、2种四环素类、2种大环内酯类、甲氧苄啶)残留的高效液相色谱串联质谱检测方法(HPLC-MS/MS)。样品提取过程中以NaF为离子交换剂,经2种提取液逐次提取,合并提取液,正己烷脱脂,萃取物经SAX-HLB固相萃取系统净化浓缩,氮吹,定容。以乙腈和0.3%甲酸为流动相,采用梯度洗脱进行液相色谱分离,以Simatone为内标物,用质谱检测器进行定性和定量分析。12种目标物的检出限为1.0~5.0 ng/g,回收率为65%~91%,相对标准偏差为0.6%~5.1%(n=4)。
A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method was developed for simultaneous determination of 12 antibiotics residues including 4 sulfonamides,3 quinolones,2 tetracyclines,2 macrolides and trimethoprim in sediments.After adding 0.4 g NaF as the ion exchanger and 200 ng trimethyl-13C3 as substitute,4 g sediment was extracted by methanol-EDTA-citrate buffer(3 ∶2 ∶1,by volume) and acetone,then degreased by n-hexane.The extract was cleaned up on a SAX-HLB solid-phase column.The target compounds were separated by liquid chromatography with gradient elution using acetonitrile-0.3% formic acid as mobile phase.The antibiotics were identified and determined by internal standard method in multiple reaction monitoring(MRM) mode.The method detected limits(LOD) of 12 compounds ranged from 1.0 ng/g to 5.0 ng/g.The recoveries of 12 compounds at three spiked levels of 50,100 and 500 ng/g ranged from 65% to 91% with relative standard deviations of 0.6%-5.1%.The method showed high sensitivity and accuracy,and was applied in the determination of 12 compounds in 17 sediment samples of Haihe River.The result indicated that except for sulfamethazine(SM 2),enrofloxacin(ENR) and erythromycin(ERY),9 antibiotics were detected with contents of 7.75-481.85 ng/g.