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超高效液相色谱-串联质谱测定菊花中11种农药残留
引用本文:徐丽萍,金来加,史陶中,马鑫,花日茂.超高效液相色谱-串联质谱测定菊花中11种农药残留[J].安徽农业大学学报,2015,42(5):813-817.
作者姓名:徐丽萍  金来加  史陶中  马鑫  花日茂
作者单位:黄山职业技术学院,屯溪,245099;安徽农业大学资源环境学院,农业部农产品贮藏保鲜质量安全风险评估实验室(合肥),农产品质量安全省级实验室, 230036;池州市农产品质量安全监测中心,池州247000;安徽农业大学资源环境学院,农业部农产品贮藏保鲜质量安全风险评估实验室(合肥),农产品质量安全省级实验室, 230036
基金项目:国家农产品质量安全风险评估项目(GJFP2015005)资助。
摘    要:建立了非茶叶类饮用植物菊花中11种农药残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。菊花样品经乙腈提取,凝胶渗透色谱(GPC)净化,收集16~38 min洗脱液,浓缩定容后采用UPLC-MS/MS在正离子模式下以多反应监测扫描方式进行监测。结果表明,GPC净化后能够有效去除杂质的干扰,11种农药3个添加水平的回收率为74.5%~115.8%,相对标准偏差(RSD)为1.8%~10.0%,决定系数(R2)在0.9990~0.9998之间。该方法操作简单、净化效果好且灵敏度高,准确度和精密度均符合农药残留分析的要求。

关 键 词:农药  多残留检测  菊花  超高效液相色谱-串联质谱

Determination of 11 pesticide residues in chrysanthemum by ultra performance liquid chromatography-tandem mass spectrometry
XU Liping,JIN Laiji,SHI Taozhong,MA Xin and HUA Rimao.Determination of 11 pesticide residues in chrysanthemum by ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Anhui Agricultural University,2015,42(5):813-817.
Authors:XU Liping  JIN Laiji  SHI Taozhong  MA Xin and HUA Rimao
Institution:Huangshan Vocational and Technical College, Tunxi 245099,Key Laboratory of Agri-Food Safety of Anhui Province, Laboratory of Quality and Safety Risk Assessment for Agro-products on Storage and Preservation ( Hefei), School of Resource and Environment, Anhui Agricultural University, Hefei 230036; Chizhou Monitoring Center of Agri-Food Safety, Chizhou 24700,Key Laboratory of Agri-Food Safety of Anhui Province, Laboratory of Quality and Safety Risk Assessment for Agro-products on Storage and Preservation ( Hefei), School of Resource and Environment, Anhui Agricultural University, Hefei 230036,Key Laboratory of Agri-Food Safety of Anhui Province, Laboratory of Quality and Safety Risk Assessment for Agro-products on Storage and Preservation ( Hefei), School of Resource and Environment, Anhui Agricultural University, Hefei 230036 and Key Laboratory of Agri-Food Safety of Anhui Province, Laboratory of Quality and Safety Risk Assessment for Agro-products on Storage and Preservation ( Hefei), School of Resource and Environment, Anhui Agricultural University, Hefei 230036
Abstract:An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method was developed for the determination of 11 pesticides in chrysanthemum. Pesticides were extracted with acetonitrile, cleaned up by GPC; eluent was collected at 16-38 min, and then separated with UPLC and detected with MS /MS in multiple reaction monitoring ( MRM) mode via positive electrospray ionization(ESI+). The results showed that it can effectively remove the interference of impurity. The average recoveries of the 11 pesticides at three fortification levels were between 74.5%-115.8%, with relative standard deviations ( RSDs) between 1.8%-10.0%, and determination coefficient (R2) between 0.9990 - 0.9998. The result indicated that this method is easy, sensitive and can achieve a good cleanup effect. The sensitivity, accuracy and precision of the method are all suitable and can meet the requirements of the multiple pesticide residues analysis.
Keywords:pesticide  multi-residue detection  chrysanthemum  ultra performance liquid chromatography- tandem mass spectrometry
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