摘要
针对土壤中抗生素污染日益严重的问题,为了促进土壤中抗生素监测技术体系及相关标准的完善,建立了一种QuEChERS结合超高效液相色谱-串联质谱(UPLC-MS/MS)的分析方法。土壤样品用10 mL 3%(体积分数,下同)氨化乙腈提取,0.2 g PSA和0.2 g无水MgSO4净化,流动相为甲醇-水(1∶1,体积比,下同),ZORBAX SB-Aq(2.1 mm×150 mm,3.5μm)色谱柱,质谱条件为电喷雾离子源(ESI)、正/负离子扫描、多反应监测(MRM)。结果表明,4种分析物在0.1~200 ng/mL范围内线性关系良好,相关系数(r)>0.999,检出限(LOD)为0.01~0.06μg/kg,定量限(LOQ)为0.05~0.19μg/kg,在3个加标水平(0.4,8.0,40.0μg/kg)下,平均回收率为87.23%~108.57%,相对标准偏差(RSD,n=5)为0.36%~6.55%。该方法准确、简便、高效、灵敏,适用于土壤中氯霉素、甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺的同步检测,可为相关部门制定相关行业标准、规范提供数据依据。
Aiming at the problem that antibiotic pollution in soil is becoming more and more serions,in order to promote the improvement of antibiotic monitoring technical system and related standards,a method of QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The soil samples were extracted with 10 mL 3%ammoniated acetonitrile(V/V),purified with 0.2 g PSA and 0.2 g anhydrous MgSO4,the mobile phase was methanol-water(1∶1,V/V),the UPLC column used in the experiment was ZORBAX SB-Aq(2.1 mm×150 mm,3.5μm),the ion source was electrospray ion source(ESI)with positive/negative ion scanning,and the detection method was multiple reaction monitoring(MRM).The results indicates that the linear relationships of the four analytes are good in the range of 0.1~200 ng/mL,with a correlation coefficients(r)higher than 0.999,the limits of detection(LOD)and the limits of quantitation(LOQ)are 0.01~0.06μg/kg and 0.05~0.19μg/kg,respectively;the average recoveries are 87.23%~108.57%at three spiked levels(0.4,8.0,40.0μg/kg),the relative standard deviations(RSDs,n=5)are 0.36%~6.55%.The method is accurate,simple,efficient and sensitive,which is suitable for the simultaneous determination of chloramphenicol,sulfoxamycin,flufenicol and its metabolite florfenicol amine in soil,and provides data basis for setting relevant standards and regulations.
作者
米旭蕾
王可
李志伟
MI Xulei;WANG Ke;LI Zhiwei(School of Chemistry and Pharmaceutical Engineering,Hebei University of Science and Technology,Shijiazhuang,Hebei 050018,China;Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang,Hebei 050011,China)
出处
《河北科技大学学报》
CAS
北大核心
2023年第2期177-185,共9页
Journal of Hebei University of Science and Technology
基金
河北省省级科技计划项目(223777116D)。
关键词
化学分析
QUECHERS
超高效液相色谱-串联质谱
土壤
氯霉素类抗生素及其代谢物
chemical analysis
QuEChERS
ultra performance liquid chromatography-tandem mass spectrometry
soil
chloramphenicol antibiotics and their metabolite
