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m-PFC净化结合高效液相色谱串联质谱法测快速测定粮谷类食品中四唑虫酰胺残留
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张可欣(1993-),女,硕士,工程师,研究方向:食品安全检测,E-mail:975351472@qq.com 通讯作者:袁列江(1973-),男,博士,教授级高级工程师,研究方向:食品质量与安全,E-mail:1277253129@qq.com

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湖南省自然科学基金项目(2022JJ90032)


m-PFC Purification Combined with HPLC-MS/MS for Rapid Determination of Tetraniliprole Residues in Grain and Cereal Foods
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    摘要:

    该研究开发了一种新型检测技术,采用改进m-PFC净化配合高效液相色谱- 质谱联用技术,实现了粮食作物样本内四唑虫酰胺残留量的快速精准检测。样品经乙腈提取,无水硫酸钠4 g,无水硫酸镁4 g去水,m-PFC HF-A净化柱净化,在Agilent Venusil MP C18(100 mm×2.1 mm,3 μm)上分离,以甲醇和水为流动相进行梯度洗脱,采用电喷雾离子化,负离子扫描,多反应监测模式(SRM)进行检测,用基质匹配外标法定量。结果显示,四唑虫酰胺在不同粮谷类食品基质下0.1~20 μg/L线性范围内决定系数(r2)均大于0.999。定量限(S/N≥10)为0.80 μg/kg。以大米、小麦、大麦、小米、大豆、绿豆、玉米、高粱为基质,该方法四唑虫酰胺在0.80、1.6、8.0 μg/kg 3个水平加标回收率范围落在84.67%至98.14%区间。对检测稳定性的评估发现,同一批次六次测量的相对标准偏差最小为0.77%,最大不超过3.36%,而不同批次间六次重复的偏差值处于0.95%到2.53%范围。该方法便捷、高效、高精度,可满足粮谷类食品中四唑虫酰胺残留的检测工作要求。

    Abstract:

    In this study, a novel detection method for rapid and accurate detection of the tetraniliprole residues in cereal crop samples was developed using improved m-PFC purification combined with HPLC-MS/MS. The samples were extracted with acetonitrile, dehydrated by 4 g of anhydrous sodium sulfate and 4 g of anhydrous magnesium sulfate, purified by m-PFC HF-A column, separated on Agilent Venusil MP C18 (100 mm×2.1 mm, 3 μm), eluted in a gradient with methanol and water as the mobile phase, iscanned with electrospray ionization and in negative ion mode, and detected by the multiple reaction monitoring (SRM) mode, and quantified by the matrix-matched external standard method. The results showed that the coefficient of determination (r2) values of tetraniliprole within the linear range (0.1~20 μg/L) and in different grain and cereal food matrices were all higher than 0.999. The limit of quantification (S/N≥10) was 0.80 μg/kg. Taking rice, wheat, barley, millet, soybeans, green beans, corn, and sorghum as the substrates, the recovery rates of tetraniliprole spiked at three levels of 0.80, 1.6 and 8.0 μg/kg ranged from 84.67% to 98.14%. The evaluation of assay stability revealed that the relative standard deviation of six measurements within the same batch (RSD, n=6) had a minimum of 0.77% and a maximum of 3.36%, whilst the relative standard deviation of six replicates between different batches (RSD, n=6) was within the range of 0.95% to 2.53%. This method is convenient, efficient and highly precise, and meets the requirements for detecting tetraniliprole residues in grain and cereal foods.

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张可欣,邓航,李政,袁列江,朱礼,黄潇宁. m-PFC净化结合高效液相色谱串联质谱法测快速测定粮谷类食品中四唑虫酰胺残留[J].现代食品科技,2025,41(8):295-303.

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  • 收稿日期:2024-06-04
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  • 在线发布日期: 2025-10-23
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