建立了固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)快速测定鸡粪中37种抗菌药物含量的方法.鸡粪经冻干制备,80％乙腈(含0.1％甲酸)提取,Oasis PRiME HLB通过式固相萃取净化后,利用UPLC-MS/MS测定抗菌药物含量.结果表明,37种抗菌药物浓度在0.40～200.0ng/mL范围内线性关系良好,相关系数(R2)大于0.996,检出限(LOD)为1 μg/kg,定量限(LOQ)为4 μg/kg.37种抗菌药物在3个浓度添加标水平(LOQ、5倍LOQ、10倍LOQ)下的回收率为63.5％～104.2％,批内相对标准偏差为1.47％～10.5％,批间相对标准偏差为2.39％～14.2％.所建立方法准确、快速、灵敏、稳定,可实现鸡粪中37种抗菌药物的同时快速测定.
Rapid Determination of 37 Antibiotics Content in Chicken Manure by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid-phase Extraction
A method for the rapid determination of 37 antibiotics content in chicken manure by ultra performance liquid chromatography-tandem mass spectrometry with solid-phase extraction has been developed.Chicken manure was prepared by freeze-drying and extracted with 80％acetonitrile(containing 0.1％formic acid),purified by Oasis PRiME HLB solid phase extraction and determined by UPLC-MS/MS.The results showed that there was a good linear relationship for the concentration of 37 antibiotics in the range of 0.40-200.0 ng/mL(R2≥0.996).Meanwhile,the LOD and LOQ were 1 μg/kg and 4 μg/kg;the recovery of 37 antibiotics ranged from 63.5％to 104.2％in three concentration levels(LOQ,5 times of LOQ,10 times of LOQ).The intra-day RSD was 1.47％-10.5％,and the inter-day RSD was 2.39％-14.2％.This method is accurate,rapid,sensitive and stable.Simultaneous and rapid determination of 37 antibiotics in chicken manure has been achieved.
Chicken manureSolid-phase extractionUltra performance liquid chromatography-tandem mass spectrometryAntibacterial drugs
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