液相色谱串联质谱法检测双孢蘑菇培养料中四环素类药物残留

采用液相色谱-串联质谱仪(LC-MS/MS)建立双孢蘑菇(Agaricus bisporus)培养料中四环素、二甲胺四环素、土霉素、甲烯土霉素、脱氧土霉素、金霉素、去甲基金霉素7种四环素类药物残留的定量分析方法。双孢蘑菇培养料以等体积Na2EDTA McIlvaine缓冲溶液(pH 4.0)和甲醇的混合液涡动,超声提取(35KHz,5min)。以HLB固相萃取柱进行净化富集,LC-MS/MS检测,结果表明:在5.0~200.0μg/L的线性范围内,7种四环素类药物的峰面积与其浓度呈良好线性关系,方法最低检出限为5.0μg/kg;在5.0、20.0、100.0μg/kg三个添加水平下,培养料基质中7种四环素类药物的回收率为80.3%~92.5%,相对标准偏差为1.6%~8.0%。该方法可以同时满足双孢蘑菇培养料中7种四环素类药物残留检测的需要。

LC-MS/MS Analysis of Residual Tetracyclines in Agaricus bisporus Compost

A quantitative analysis method was established for detecting 7 residual tetracyclines (tetracycline,minocycline,oxytetracycline,metacycline,doxycycline,chlortetracycline,and demeclocycline) in Agaricus bisporus compost by LC-MS/MS.Compost was first extracted twice in a mixture of Na2 EDTA McIlvaine buffer (pH 4.0) and methanol(1∶1,v∶v)by vortex and ultrasonic,and then extracts were concentrated by a HLB solid-phase extraction column before LC-MS/MS analysis.The results turned out that under a concentration range of 5.0～200.0 μg/L,the integration areas of 7 tetracycline antibiotics were in good linear correlation with their corresponding concentrations,and the detection limit was 5.0 μg/kg.The recovery rates of 7 tetracyclines ranged between 80.3％ and 92.5％ with relative standard deviations between 1.6％ and 8.0％ under concentrations at 5.0,20.0 and 100.0 μg/kg.