通过式固相萃取柱/超高效液相色谱-串联质谱法同时测定水产养殖沉积物中磺胺类、喹诺酮类、四环素类22种抗生素兽药残留  

Simultaneous Determination of Sulfonamides,Quinolones and Tetracycline 22 Antibiotics Residues in Aquaculture Sediments Using Solid-Phase Extraction Column/ultra-High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：赵天珍 宋海霞 何国成 梁莹 宋长江 ZHAO Tian-zhen;SONG Hai-xia;HE Guo-cheng;LIANG Ying;SONG Chang-jiang(Zhongshan Quality Safety&Inspection Institute of Agricultural Products,Zhongshan 528400,China)

机构地区：[1]中山市农产品质量安全检验所,广东中山528400

出　　处：《安徽化工》2024年第2期170-176,共7页Anhui Chemical Industry

摘　　要：目的:建立了同时测定水产养殖沉积物中22种抗生素的通过式固相萃取柱/超高效液相色谱-串联质谱法。方法:样品用8 mL EDTA-Mcllvaine-乙腈=4∶4超声提取,提取液过HLB通过式固相柱净化,UPLC-MS/MS检测,基质工作曲线和同位素内标法同时定量。结果:在2.00~100μg/L范围内,22种抗生素的线性关系良好,相关系数均大于0.998。在10μg/kg、50μg/kg、100μg/kg这3个添加水平下,重复测定6次,回收率在60.3%~109.7%,相对标准偏差为1.2%~13.2%,符合GB/T 27404—2008对回收率和精密度的要求。结论:该方法高效快捷,准确可靠,适用于沉积物中抗生素类药物的快速测定。Objective:The method for simultaneous determinatiom of 22 antibiotics residues in sediment from aquaculture environment by using ultra high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)in combination with pass-through column was established.Method:The samples were extracted by ultrasonic with 8 mL EDTA-Mcllvaine and acetonitrile equal to 4∶4,and purified by HLB pass-through solid phase column.After purification,the samples were analyzed by UPLC-MS/MS,and the samples were quantified simultaneous by matrix working curve and isotope internal standard method.Results:There was a good linear relationship in the range of 2.00~100μg/L,with R greater than 0.998.The recoveries were in the range of 60.3%~109.7%,and the RSD was in the range of 1.2%~13.2%at 10μg/kg,50μg/kg and 100μg/kg supplemental levels for six times,which met the requirements of recoveries and precision for GB/T 27404—2008.Conclusion:The method is efficient,fast,accurate and reliable.It is suitable for the fast determination of the antibi-otics in sediment.

关 键 词：超高效液相色谱-串联质谱法 沉积物 抗生素 基质工作曲线 同位素内标 

分 类 号：O657.63[理学—分析化学]