摘要
目的建立了分散固相萃取(d-SPE)-气相色谱-三重四级杆串联质谱法(GC-MS/MS)测定代用茶中14种农药残留的分析方法。方法用乙腈提取样品中待测组分,提取物经N-丙基乙二胺(PSA)分散固相萃取净化后,以DB-5MS柱(30 m×0.25 mm,0.25μm)进行色谱分离,采用GC-MS/MS在多反应监测(MRM)模式下检测,外标法定量。结果在一定的含量范围内线性关系良好,相关系数r≥0.999,方法定量限4~40μg/kg。以空白基质进行3个水平(20、40和200μg/kg)的加标回收实验,平均回收率为65.6%~116.6%,相对标准偏差(RSDs)为1.5%~15.7%(n=6)。结论该方法简单快速、灵敏度高、选择性好,可满足常用代用茶中农药多残留同时分析的要求。
Objective The method was established for determination 14 kinds of psticide residues in substitutional tea using gas chromatography-triple quadrupole mass spectrometry（ GC-MS/MS） for instrument method and dispersive solid-phase extraction（ dSPE） for sample preparation.Methods The samples extracted with acetonitrile,and purified by N-propyl ethlene diamine（ PSA）,the extracts were separated on DB-5MS column（ 30 m × 0.25 mm,0.25 μm） with programmed temperature and determined by GCMS/MS in multi-reaction monitoring（ MRM） model.The external standard method was applied to quantify the pesticides.Results The method showed a good linearity（ r ≥0.999） in certain ranges for 14 kinds of pesticides.The limits of quantification（ LOQ）were 4-40 μg/kg.The average recoveries range were 65.6%-116.6% in three add levels of 20,40 and 200 μg/kg,and relative standard deviations（ RSD S） of 1.5%-15.7%（ n = 6）.Conclusion This method is simple,fast,sensitive,selective and can satisfy the request of simultaneous analysis of multiple pesticide residues in substitutional tea.
作者
李晔
赵丹莹
郭爱华
温雅
李堃
吴国华
Li Ye;Zhao Danying;Guo Aihua;Wen Ya;Li Kun;Wu Guohua(Beijing Xicheng District Center for Disease Control and Prevention,Beijing 100120,China)
出处
《卫生研究》
CAS
CSCD
北大核心
2018年第4期621-627,共7页
Journal of Hygiene Research
