摘要
建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)快速检测洛党参中乙基多杀菌素-J(XDE-175-J)和乙基多杀菌素-L(XDE-175-L)残留的方法。样品经乙腈提取,乙二胺-N-丙基硅烷和石墨化炭黑净化后,外标法定量。结果表明,XDE-175-J和XDE-175-L的峰面积与其质量浓度分别在0.075~75μg/L和0.025~25μg/L范围内,呈良好线性关系(r2>0.990);在0.375、3.75、75μg/kg加标水平下,XDE-175-J的平均回收率为88.4%~113.5%,相对标准偏差(RSD,n=5)为2.0%~4.2%;在0.125、1.25、25μg/kg加标水平下,XDE-175-L的平均回收率为84.4%~99.5%,RSD(n=5)为2.5%~4.9%。乙基多杀菌素的定量下限(LOQ)为0.375μg/kg(XDE-175-J)和0.125μg/kg(XDE-175-L)。该方法简便、快捷,灵敏度高,回收率和重复性良好,能满足农药残留检测技术要求,可用于大量洛党参样品中乙基多杀菌素的残留分析。
An ultra-high performance liquid chromatography-tandem mass spectrometric（UHPLC-MS/MS） method was established for the determination of spinetoram residues,XDE-175-J and XDE-175-L in Radix Gotonopsic Tongshen Otiv. The samples were exacted with acetonitrile,and purified with primary secondary amine and graphitized carbon black. The target compounds were quantified by the external standard method. There were good linearities for the peak areas of XDE-175-J and XDE-175-L in the concentration ranges of 0. 075-75 μg/L and 0. 025-25 μg/L,respectively. The average recoveries for XDE-175-J and XDE-175-L at the spiked levels of0. 375,3. 75,75 μg/kg and 0. 125,1. 25,25 μg/kg were in the ranges of 88. 4%-113. 5% and84. 4%-99. 5%,with relative standard deviations（RSDs） of 2. 0%-4. 2% and 2. 5%-4. 9%,respectively. The limits of quantitation（LOQs） for XDE-175-J and XDE-175-L were 0. 375μg/kg and 0. 125 μg/kg,respectively. With the advantages of simplicity,rapidness and convenience,the method could meet the requirements for pesticide residues analysis,and be applied in the rapid detection of spinetoram residues in Radix Gotonopsic Tongshen Otiv.
作者
李刚
秦樊鑫
张盈
龙家寰
魏进
LI Gang;QIN Fan-xin;ZHANG Ying;LONG Jia-huan;WEI Jin(Guizhou Provincial Key Laboratory for Information Systems of Mountainous Areas and Protection of Ecological Environment,Guizhou Normal University,Guiyang 550001,China;Institute of Plant Protection,Guizhou Academy of Agricultural Science,Guiyang 550006,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第7期834-838,共5页
Journal of Instrumental Analysis
基金
贵州五种特色果蔬病虫害绿色防控技术体系服务企业行动计划(黔科合服企[2015]4012号)
洛党参重要病虫害无公害防治关键技术研究与应用示范(道科合[2014]07号)
关键词
乙基多杀菌素
超高效液相色谱-串联质谱(UHPLC-MS/MS)
洛党参
残留检测
spinetoram
ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS ）
Radix Gotonopsic Tongshen Otiv.
residues determination
