摘要
建立了QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定土壤中60种农药和24种抗生素的分析方法。样品用Na2EDTA-Mcllvaine缓冲液(pH 7.20)和5%(体积分数)甲酸乙腈溶液提取,经十八烷基键合硅胶(C18)和N-丙基乙二胺(PSA)净化。采用ACQUITY UPLC BEH C_(18)柱(2.1 mm×100 mm,1.7μm)分离,在多反应监测(MRM)模式下检测,基质匹配标准溶液外标法定量。结果表明,84种目标化合物在各自质量浓度范围内线性关系良好,相关系数(r2)不小于0.990。除甲基硫菌灵、多西环素和金霉素的定量下限(LOQ)为0.1 mg/kg外,其余化合物的LOQ均为0.01 mg/kg。84种目标化合物在不同加标水平下的回收率为60.9%~118%,相对标准偏差(RSD,n=5)为0.38%~22%。该方法操作简便、灵敏度高、准确度好,适用于土壤中多种农药和抗生素的检测。
An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with QuEChERS was established for the simultaneous determination of 60 pesticides and 24 anti⁃biotics in soil.The samples were extracted with Na2EDTA-Mcllvaine buffer solution(pH 7.20)and acetonitrile solution containing 5.0%(by volume)formic acid,then purified with octadecyl silane(C18)and primary secondary amine(PSA).Analytes were separated on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm,1.7μm),then detected under multiple reaction monitoring(MRM)mode,and quantified by matrix-matched standard solutions and external standard method.Results showed that there existed good linear relationships for 84 compounds in their respective concentration ranges,with correlation coefficients(r2)not less than 0.990.The limits of quantitation(LOQs)of 81 compounds were 0.01 mg/kg except for LOQs of thiophanate-methyl,doxycycline and chlortetra⁃cycline were 0.1 mg/kg.The recoveries ranged from 60.9%to 118%,with relative standard devia⁃tions(RSDs,n=5)of 0.38%-22%.This method is simple,sensitive and accurate,and it could be applied to the determination of pesticides and antibiotics in soil.
作者
杨艳梅
李晋栋
秦曙
YANG Yan-mei;LI Jin-dong;QIN Shu(Shanxi Center for Testing of Functional Agro-products,Shanxi Agricultural University,Taiyuan 030031,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第7期808-816,共9页
Journal of Instrumental Analysis
基金
山西省重点研发计划项目(201903D211011-5,202102140601018)。
关键词
QUECHERS
超高效液相色谱-串联质谱
土壤
农药
抗生素
QuEChERS
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
soil
pesticides
antibiotics
