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粮食中玉米赤霉烯酮含量测定的前处理方法优化

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优化GB 5009.209-2016 高效液相色谱法前处理过程,建立新的粮食中玉米赤霉烯酮含量的高效液相色谱测定方法.样品经乙腈-水(V乙腈:V水=4∶1)调速振荡器提取,免疫亲和柱富集净化,甲醇洗脱后,直接用水稀释定量至 2.00 mL,采用 C18 反相色谱柱(150 mm×4.6 mm,5.0 μm),在 10~500 ng/mL的质量浓度范围内线性关系良好,其相关系数R2 为0.999,检出限(LOD)和定量限(LOQ)分别为3.8 μg/kg、12.8 μg/kg,3 个浓度水平加标回收率为 94.3%~106.3%,精密度为 0.8%~6.1%,连续 4 天的基质加标回收率为96.7%~104.8%,日间精密度为 0.8%~4.3%,高效液相色谱可以很好地对粮食中玉米赤霉烯酮进行快速准确定量分析.经验证该方法与国标方法检测结果无显著性差异.与国标相比,尤其是本方法通过去除氮吹、省去流动相复溶步骤可实现快速、简便、批量检测,提高了工作效率.
Optimization of pre-treatment method for determining the content of zearalenone in food
Optimization of the pretreatment process of high-performance liquid chromatography in GB 5009.209-2016,and the establishment of a new high-performance liquid chromatography method for the determination of Zearalenone in grain.The samples were extracted by(Vacetonitrile:Vwater=4∶1)speed-regulating oscillator,enriched and purified by an immunoaffinity column,and eluted with methanol.The eluate was then diluted and quantified to 2.00 mL with water directly,analyzed using a C18 reversed-phase chromatographic column(150 mm×4.6 mm,5.0μm).The linear relation-ship was good within the mass concentration range of 10-500 ng/mL,with a correlation coefficient(R2)of 0.999.The detection limit(LOD)was 3.8 μg/kg,and the quantitative limit(LOQ)was 12.8 μg/kg,the recoveries were 94.3%~106.3%,the precision was 0.8%~6.1%,the recoveries were 96.7%~104.8%,the daytime precision was 0.8%~4.3%.The high-performance liquid chromatography can be used for rapid and accurate quantitative analysis of Zearalenone in grains.Compared with the national standard method,there was no significant difference.Especially,the method can realize rapid,simple,and batch detection by removing nitrogen blowing and removing the steps of mobile phase re-dissolving,thus improving the working efficiency.

grainszearalenonehigh-performance liquid chromatographyimmunoaffinitypretreatments

唐陵辉、杨振飞

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永州市食品质量安全监督检测检验中心,湖南 永州 425000

粮食 玉米赤霉烯酮 高效液相色谱 免疫亲和柱 前处理

2024

粮食科技与经济
湖南省粮食经济科技学会 中诸粮管理总公司湖南分公司

粮食科技与经济

影响因子:0.505
ISSN:1007-1458
年,卷(期):2024.49(2)