Sin-QuEChERS Nano-UPLC-MS/MS检测大米中甲氨基阿维菌素苯甲酸盐残留
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1.怀化市疾病预防控制中心,湖南 怀化 418000;2.长沙理工大学化学与医药工程学院,湖南 长沙 410114

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黄子杰(1989—),男,怀化市疾病预防控制中心助理研究员,硕士。E­mail:284278972@qq.com

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怀化市科技计划创新项目(编号:2021R3120)


Determination of residual emamectin benzoate in rice by Sin-QuEChERS Nano-UPLC-MS/MS
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1.Huaihua Center for Disease Control and Prevention, Huaihua, Hunan 418000, China;2.School of Chemistry and Pharmaceutical Engineering, Changsha University of Science and Technology, Changsha, Hunan 410114, China

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    摘要:

    目的 建立一种新的Sin-QuEChERS Nano-三重四极杆液质联用仪(UPLC-MS/MS)检测大米中甲氨基阿维菌素苯甲酸盐(甲维盐)残留的方法。方法 样品经0.1%甲酸—乙腈提取后,N-丙基乙二胺(PSA)和多壁碳纳米管(MWCNTs)填料净化,以0.1%甲酸水和乙腈为流动相梯度洗脱,经C18色谱柱分离,采用三重四极杆液质联用仪测定。结果 甲维盐的定量限为0.001 5 mg/kg,方法检出限为0.000 5 mg/kg。甲维盐在1~100 ng/mL质量浓度范围内呈良好的线性关系,相关系数>0.999 5。在2,10,50 μg/kg添加水平下,甲维盐的平均回收率为86.9%~110.2%,相对标准偏差为0.98%~7.21%。结论 该方法高效简便、稳定性好、灵敏度高,适用于大米中甲维盐的检测。

    Abstract:

    Objective To establish a new Sin-QuEChERS nano-triple quadrupole liquid chromatography-mass spectrometry (UPLC-MS/MS) method for detecting emamectin benzoate residues in rice.Methods After extraction with 0.1% formic acid-acetonitrile, the sample is purified with N-primary secondary amine (PSA) and multi-walled carbon nanotube (MWCNTs) fillers. The mobile phase is a gradient elution of 0.1% formic acid water and acetonitrile. Separation is performed using a C18 chromatographic column, and the detection is carried out using a triple quadrupole liquid chromatography-tandem mass spectrometry system.Results The quantification limit of emamectin benzoate is 0.001 5 mg/kg, and the detection limit of the method is 0.000 5 mg/kg. A good linear relationship is observed for emamectin benzoate in the concentration range of 1~100 ng/mL, with a correlation coefficient greater than 0.999 5. At 2, 10, and 50 μg/kg spiking levels, the average recovery rate of emamectin benzoate is 86.9%~110.2%, with a relative standard deviation of 0.98%~7.21%.Conclusion This method is efficient, simple, stable, and highly sensitive, making it suitable for detecting emamectin benzoate in rice.

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罗宽能,黄子杰,黄朋勉,等.Sin-QuEChERS Nano-UPLC-MS/MS检测大米中甲氨基阿维菌素苯甲酸盐残留[J].食品与机械,2025,41(8):61-65.
LUO Kuanneng, HUANG Zijie, HUANG Pengmian, et al. Determination of residual emamectin benzoate in rice by Sin-QuEChERS Nano-UPLC-MS/MS[J]. Food & Machinery,2025,41(8):61-65.

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  • 收稿日期:2024-09-11
  • 最后修改日期:2025-03-21
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  • 在线发布日期: 2025-09-25
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