CAJ | 학술논문

采用高效液相色谱-串联质谱法( HPLC-MS/MS),同时测定有机肥料中3类9种抗生素(土霉素、四环素、金霉素、强力霉素、青霉素G和普鲁卡因青霉素、磺胺嘧啶、磺胺二甲基嘧啶、磺胺噻唑)残留,对于有机肥料中抗生素残留的快速检测具有重要的意义。样品用Na2 EDTA-McIlvaine缓冲液超声振荡提取后,采用固相萃取小柱净化,高效液相色谱-串联质谱法检测,标准曲线外标法定量。采用多反应监测模式检测,除负离子扫描青霉素G外其他均用正离子扫描。方法在0．1、0．5、1．0 mg/kg 添加水平下,样品平均回收率为63．1%~93．4%；相对标准偏差为1．7%~9．5%；四环素类药物的方法检出限均可达到0．05 mg/kg,磺胺类和青霉素类药物的检出限可达0．02 mg/kg。本方法简便、快速,重现性良好,可用于有机肥料样品中抗生素残留的快速确证检测。
채용고효액상색보-천련질보법( HPLC-MS/MS),동시측정유궤비료중3류9충항생소(토매소、사배소、금매소、강력매소、청매소G화보로잡인청매소、광알밀정、광알이갑기밀정、광알새서)잔류,대우유궤비료중항생소잔류적쾌속검측구유중요적의의。양품용Na2 EDTA-McIlvaine완충액초성진탕제취후,채용고상췌취소주정화,고효액상색보-천련질보법검측,표준곡선외표법정량。채용다반응감측모식검측,제부리자소묘청매소G외기타균용정리자소묘。방법재0．1、0．5、1．0 mg/kg 첨가수평하,양품평균회수솔위63．1%~93．4%；상대표준편차위1．7%~9．5%；사배소류약물적방법검출한균가체도0．05 mg/kg,광알류화청매소류약물적검출한가체0．02 mg/kg。본방법간편、쾌속,중현성량호,가용우유궤비료양품중항생소잔류적쾌속학증검측。
A sensitive high performance liquid chromatography-tandem mass spectrometric ( HPLC-MS/MS) method has been developed for simultaneous determination of nine antibiotics residues ( oxytetracycline, tetracycline, chlortetracycline, doxy-cycline, penicillin G, procaine penicillin, sulfadiazine, sulfadimidine and sulfathiazole) in organic fertilizer. It is of great significance to the rapid detection of antibiotic residues in organic fertilizers. In this paper, the samples were extracted by ul-trasonic oscillation with Na2 EDTA-McIlvaine buffer solution, then extracts was cleaned up by the Strata SDB-L solid phase ex-traction column. The contents of antibiotics were determined by high performance liquid chromatography-tandem mass spectrom-etry and calculated by external standard method. Multiple reactions monitoring mode was utilized. Most analytes were scanned by positive-ion electrospray ionization except penicillin G. Average recoveries of the nine analytes were in the range of 63. 1%to 93. 4% at spiking levels of 0. 1, 0. 5 and 1. 0 mg/kg. Relative standard deviations were between 1. 7% and 9. 5%. The method detection limits of tetracycline antibiotics were 0. 05 mg/kg, and the method detection limits of sulfonamides and peni-cillins were 0. 02 mg/kg. The method was convenient, fast, with good reproducibility, and could be used to simultaneously and fast confirm multi-residue of antibiotics in organic fertilizer.