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作 者:黄子杰 黄朋勉 罗宽能 向忠平 张洪刚[2] HUANG Zijie;HUANG Pengmian;LUO Kuanneng;XIANG Zhongping;ZHANG Honggang(Huaihua Center for Disease Control and Prevention,Huaihua,Hunan 418000,China;School of Chemistry and Chemical Engineering,Changsha University of Science&Technology,Changsha,Hunan 410114,China)
机构地区:[1]怀化市疾病预防控制中心,湖南怀化418000 [2]长沙理工大学化学化工学院,湖南长沙410114
出 处:《食品与机械》2024年第1期63-67,共5页Food and Machinery
基 金:怀化市科技计划创新项目(编号:2021R3120);湖南省教育厅科学研究项目(编号:湘教通[2020]264号)。
摘 要:目的:建立一种新的QuEChERS-超高效液相色谱—串联质谱(UPLC-MS/MS)检测大米中氯虫苯甲酰胺和五氟磺草胺的残留方法。方法:样品经0.2%甲酸—乙腈提取后,N-丙基乙二胺(PSA)和石墨化碳黑(GCB)填料净化,以0.2%甲酸水—乙腈为流动相梯度洗脱,经C 18色谱柱分离,采用UPLC-MS/MS测定。结果:氯虫苯甲酰胺和五氟磺草胺的定量限(LOQ)均为0.004 mg/kg,方法检出限(LOD)均为0.001 mg/kg。两种待测农药在0.002~0.5 mg/L质量浓度范围内呈良好的线性关系,其相关系数均在0.993以上。在0.05,0.1,0.5 mg/kg添加水平下,两种待测农药的平均回收率为86%~110%;相对标准偏差(RSD)为1.5%~6.1%。结论:该方法高效简便、稳定性好、灵敏度高,适用于大米中氯虫苯甲酰胺和五氟磺草胺的检测。Objective:To establish a new QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the detection of chlorantraniliprole and penoxsulam residues in rice.Methods:After the sample was extracted with 0.2%formic acid-acetonitrile,purified with N-propylethylenediamine(PSA)and graphitized carbon black(GCB)packing,0.2%formic acid water and acetonitrile were used as mobile phases for gradient elution,and then subjected to C 18 chromatography.UPLC-MS/MS was used to column separation and determination.Results:The limits of quantification(LOQ)of chlorantraniliprole and penoxsulam were both 0.004 mg/kg,and the method detection limits(LOD)were both 0.001 mg/kg.Chlorantraniliprole and penoxsulam had a good linear relationship in the range of 0.002~0.5 mg/L,and their coefficient was greater than 0.993.At the addition levels of 0.05,0.1,and 0.5 mg/kg,the average recovery rates of chlorantraniliprole and penoxsulam were 86%to 110%with the relative standard deviations(RSD)of 1.5%to 6.1%.Conclusion:This method is efficient and simple,has good stability and high sensitivity,and is suitable for the detection of chlorantraniliprole and penoxsulam in rice.
关 键 词:QUECHERS 氯虫苯甲酰胺 五氟磺草胺 大米 残留
分 类 号:TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]
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