高效液相色谱-串联质谱同时测定有机肥料中9种抗生素药物残留

Determination of nine antibiotics residues in organic fertilizer by high performance liquid chromatography-tandem mass spectrometry

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Na2EDTA-Mc Ilvaine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。

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,doxycycline,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 ultrasonic oscillation with Na2EDTA-Mc Ilvaine buffer solution,then extracts was cleaned up by the Strata SDB-L solid phase extraction column. The contents of antibiotics were determined by high performance liquid chromatography-tandem mass spectrometry 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 penicillins 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.