YANG Jing,WU Yan,NIU Yan,et al.Determination of Spirotetramat and Its Metabolites Residues in Lycium Fruit Based on the HPLC-MS/MS Technology[J].Northern Horticulture,2020,44(24):113-118.[doi:10.11937/bfyy.20200126]
基于HPLC-MS/MS技术测定枸杞中螺虫乙酯及其代谢物残留的方法
- Title:
- Determination of Spirotetramat and Its Metabolites Residues in Lycium Fruit Based on the HPLC-MS/MS Technology
- Keywords:
- Lycium; spirotetramat; metabolites; test
- 文献标志码:
- A
- 摘要:
- 以枸杞果实为试材，利用超高效液相色谱串联质谱技术，对枸杞果实中螺虫乙酯及其代谢物（螺虫乙酯烯醇、羟苯螺虫乙酯酮、螺虫乙酯烯醇葡萄糖苷和单羟基螺虫乙酯）进行检测。枸杞样品用0.1%甲酸乙腈提取，N-丙基乙二胺(PSA)和石墨化炭(GCB)净化后，采用超高效液相色谱-三重四级杆质谱联用仪检测，外标法定量。结果表明：枸杞鲜果中螺虫乙酯及其代谢物的添加回收率为79.8%～116.1%，相对标准偏差为3.9%～16.6%；枸杞干果中螺虫乙酯及其代谢物的添加回收率为77.8%~119.2%，相对标准偏差为2.9%~15.1%。该方法的回收率、精密度均较好，符合农药残留分析的要求。
- Abstract:
- Lycium fruits were used as experimental materials.A residue analytical method (HPLC-MS/MS) has been developed for the determination of spirotetramat and its metabolites (spirotetramat-enol,spriotetramat-keto-hydroxy,spriotetramat-enol-glucoside,spirteteramat-mono-hydroxy) in Lycium by sample screening and preparation methmazine in Lycium were studied by means of high performance liquid chromatography mass spectrometry (HPLC-MS/MS).The samples of Lycium fruit were extracted with 0.1% acetonitrile formate,purified with n-propyl ethylenediamine(PSA) and graphitized carbon(GCB),and then detected by HPLC-MS/MS.The results showed that the average recovery of residues in fresh fruit of Lycium raged from 79.8% to 116.1% with RSD of 3.9%-16.6%.The average recovery of residues in dry fruit of Lycium raged from 77.8 to 119.2% with RSD of 2.9%-15.1%.The recovery rate and precision of the method are good,which meet the requirements of pesticide residue analysis.
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备注/Memo
第一作者简介：杨静(1986-)，女，硕士，助理研究员，现主要从事农产品农药残留检测方法等研究工作。E-mail：289184175@qq.com.责任作者：王晓菁(1972-)，女，硕士，研究员，现主要从事农产品质量标准等研究工作。E-mail：niuyan98@163.com.基金项目：农业行业标准制修订资助项目(181821301092372)。收稿日期：2020-01-08