首页|QuEChERS-UPLC-MS/MS法同时测定枸杞子中15种新烟碱类农药及代谢产物残留量

QuEChERS-UPLC-MS/MS法同时测定枸杞子中15种新烟碱类农药及代谢产物残留量

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建立了枸杞中15种新烟碱类农药及其代谢产物残留量的QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法.采用Agilent Zorbax HILIC色谱柱(100 mm×4.6 mm,3.5 µm),以0.1%甲酸(含5 mmol/L甲酸铵)-乙腈为流动相,梯度洗脱,柱温为35℃,流速0.3 mL/min.电离方式为电喷雾正离子模式(ESI+),使用多反应监测模式(MRM)进行定量分析.结果显示,15种新烟碱类农药及代谢产物在考察浓度范围内呈良好的线性关系(r>0.996),方法检出限(LOD)为0.001~0.005 mg/kg,方法定量限(LOQ)为0.003~0.020 mg/kg,平均回收率为77.3%~113.6%,相对标准偏差(RSD)为3.4%~11%.所建立的方法能够对枸杞子中新烟碱类农药及其代谢产物残留进行定量分析.
Simultaneous determination of 15 neonicotinoid pesticide and metabolite residues in Lycium by ultra-performance liquid chromatography-tandem mass spectrom-etry coupled with QuEChERS
A QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous determination of 15 neonicotinoid pesticide and metabolite residues in Lycium.An Agilent Zorbax HILIC column(100 mm×4.6 mm,3.5 µm)with 0.1%formic acid(containing 5 mmol/L ammonium formate)-acetonitrile as the mobile phase in a gradient elution was applied for the separation,with a flow rate of 0.3 mL/min and a column temperature of 35℃.Multiple-reaction monitoring(MRM)scanning was employed for the quantification with switching electrospray ion source polarity in positive mode(ESI+).The linear relationships of 15 neonicotinoid pesticides and metabolites were good in their concentration ranges(R2>0.996).The limit of detection(LOD)and limit of quantitation(LOQ)were in the ranges of 0.001‒0.005 mg/kg and 0.003‒0.020 mg/kg,respectively.The recoveries ranged from 77.3%to 113.6%,and the relative standard deviations(RSDs)ranged from 3.4%to 11%.The method could meet the requirements for simultaneous detection of 15 neonicotinoid pesticides and their metabolites in Lycium.

Lyciumultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)neonicotinoid pesticidesmetabolites

高萌、贺凯、张家萌、刘潇然、马玲

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宁夏回族自治区药品检验研究院,国家枸杞产品质量检验检测中心(宁夏),宁夏药品监督管理局中药质量控制重点实验室,宁夏回族自治区药品质量控制与评价重点实验室,银川 750004

枸杞子 超高效液相色谱-串联质谱(UPLC-MS/MS) 新烟碱类农药 代谢产物

2025

分析试验室
北京有色金属研究总院 中国分析测试协会

分析试验室

北大核心
影响因子:1.171
ISSN:1000-0720
年,卷(期):2025.44(1)