固相萃取-超高效液相色谱串联质谱法同时检测禽畜粪便中多种抗生素残留  

Simultaneous Determination of Residual Antibiotics in Livestock Manure by Solid Phase Extraction-Ultra-high Performance Liquid Chromatography Tantem Mass Spectrometry

作　　者：万位宁[1] 陈熹[1] 居学海[2] 母全华[1] 王冲[1] 毛大庆[3] 罗义[1] 

机构地区：[1]南开大学环境科学与工程学院环境污染过程与基准教育部重点实验室,天津300071 [2]农业部产地环境与农产品安全重点开放实验室农业部环境保护科研监测所,天津300191 [3]天津大学环境科学与工程学院,天津300072

出　　处：《分析化学》2013年第7期993-999,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21037002;31070333;31270542);国家环保公益项目(No.201309031);国家级大学生"百项创新"项目资助

摘　　要：建立了固相萃取-超高效液相色谱串联质谱(SPE-UPLC/MS/MS)同时测定禽畜粪便中6种磺胺类(SAs)、4种四环素类(TCs)、3种氟喹诺酮类(FQs)、3种大环内酯类(MACs)以及1种硝基呋喃类(NFs)抗生素残留的方法。样品分别由McIlvaine-Na2EDTA缓冲液和有机混合提取液逐次超声提取,合并提取液,以正己烷去脂,过SAX-HLB固相萃取系统富集净化,经氮吹、定容后,以乙腈和0.1%甲酸-水溶液为流动相进行UPLC/MS分离检测,内标法定量。在0.1～1000μg/kg(Dry weight)浓度范围内,所有目标物标准曲线R2均大于0.99,样品加标回收率在42.3%～79.6%之间,相对标准偏差为1.4%～5.4%。方法检出限为0.1～2.0μg/kg,定量下限为0.3～6.6μg/kg。应用本方法检测华北地区多个禽畜养殖基地粪便样品32份,所有抗生素均有不同程度的检出,最高检出浓度为金霉素125μg/kg。A ultra-high performance liquid chromatography tandem mass spectrometric （UPLC-MS/MS） method was developed for the simultaneous determination of various antibiotics residues including 6 sulfonamides（SAs）, 4 tetracyclines （TCs）, 3 quinolones （FQs）, 3 macrolides （MACs） and 1 nitrofuran （NFs） in livestock manures. The samples were extracted with Mcllvaine-Na2EDTA buffer and organic mixed extract solution by ultrasonic extraction, and then degreased by n-hexane. The extract was cleaned upon a SAX-HLB solid phase column. After drying the extract under a gentle stream of N2 and reconstituting the dried residue, the target compounds were analyzed by ultra-high performance liquid chromatography with gradient elution using a cetonitrile-0.1% formic acid as mobile phase. The antibiotics were identified and determined by internal standard method. In the concentration range of 0.1-1000 μg/kg （dry weight）, R2 of calibration curve for all the objects was above 0.99. The detected limits （LOD） ranged from 0.1 ng/g to 2.0 μg/kg, limit of quantification （LOQ） ranged from 0.3 to 6.6 μg/kg. The recoveries of target compounds at three spiked levels ranged from 42.3% to 79.6% with relative standard deviations of 1.4% -5.4%. The method was applied on the determination of residual antibiotics in 32 manure samples collected from several animal feeding operations in Northen China. The results indicated that all of the selected antibiotics were detected at different levels, in which the highest concentration was chlortetracycline with 125 mg/kg.

关 键 词：粪便 抗生素 残留 固相萃取-超高效液相色谱串联质谱(SPE-UPLC MS MS) 

分 类 号：S859.84[农业科学—临床兽医学]