复合型固相萃取-离子对反相液相色谱法测定蔬菜中的灭蝇胺残留
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(广州市食品检验所 广州 511400)

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王成龙(1991—),男,学士,工程师

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广州市科技计划项目(202102080615);广州市市场监督管理局科技创新项目(2022kj38)


Determination of Cyromazine Residues in Vegetables by Composite Solid-phase Extraction and Reverse Phase ion-pair High Performance Liquid Chromatography
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(Guangzhou Institute for Food Inspection, Guangzhou 511400)

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    摘要:

    为建立复合型固相萃取-离子对反相液相色谱(IS-RPLC)快速、准确测定蔬菜中灭蝇胺残留的方法,采用碳酸氢铵溶液多次超声萃取方式提取目标物,经复合型固相萃取小柱净化,结合离子对反相液相色谱系统分离、测定。在0.1~2 μg/mL线性范围呈线性(相关系数大于0.998),方法检出限(LOD)达0.012 mg/kg,满足各类蔬菜基质对灭蝇胺残留的监管判定要求。通过加标验证,回收率在77.7%~87.0%范围,相对标准偏差(RSD)为1.6%~3.7%。方法解决了灭蝇胺萃取回收率低、净化困难的问题,结合离子对试剂的C8色谱柱反相保留,使灭蝇胺出峰良好,抗干扰强。

    Abstract:

    A rapid and accurate method for the determination of cyromazine residues in vegetables by composite solid-phase extraction and reversed phase ion-pair liquid chromatography(IS-RPLC) was established. The target was extracted by multiple ultrasonic extraction with ammonium bicarbonate solution, purified by composite solid-phase extraction column, and separated and determined by IS-RPLC. The calibration curve showed good linearity in the range of 0.1~2 μg/mL with the correlation coefficient greater than 0.998, and the limit of detection (LOD) of the method reaches 0.012 mg/kg, which can meet the regulatory and judgment requirements for the residue of cyromazine. Recovery experiments show that the recovery range is 77.7%~87.0%, and the relative standard deviation (RSD) is 1.6%~3.7%. The problems of low extraction recovery and difficult purification in the determination of cyromazine were effectively solved. The chromatographic peak shape of cyromazine which separated by C8 column combining with the ion-pair reagent was sharp and anti-interference.

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王成龙,刘佳,王宇,黄小清,林泽珊,赵金利,谭锦萍,黄松.复合型固相萃取-离子对反相液相色谱法测定蔬菜中的灭蝇胺残留[J].中国食品学报,2022,22(9):285-292

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  • 收稿日期:2022-05-09
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  • 在线发布日期: 2022-10-26
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