摘要
建立了固相萃取高效液相色谱串联质谱法测定九华黄精中26种农药残留的方法。试样采用乙腈提取,所得提取液经分散固相萃取净化后,用超高效液相色谱串联质谱检测,以外标法定量。26种农药的标准曲线在0.002~0.200μg·mL^(-1)线性良好,相关系数均在0.996以上,方法检出限在0.01~0.05 mg·kg^(-1),定量限在0.03~0.15 mg·kg^(-1)。不同加标水平的平均回收率在62.8%~108.6%,回收率相对标准偏差范围在0.5%~9.1%(n=6)。经优化后的前处理方法,操作简便,重现性较好,回收率能够满足要求,可提高检测效率,降低检测成本。
A method was developed for the determination of 26 pesticide residues in Polygonatum cyrtonema by ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by acetonitrile,and the extracted liquid was purified by dispersed solid phase extraction,detected by HPLC-MS/MS,and quantitative analysed by external standard method.The standard curves of 26 pesticides had good linearity in the concentration range of 0.002~0.200μg·mL^(-1),and the correlation coefficients were all above 0.996.The detection limit of the method is 0.01~0.05 mg·kg^(-1),and the quantitative limit is 0.03~0.15 mg·kg^(-1).The average recovery was 62.8%~108.6%,and the relative standard deviation of recovery was 0.5%~9.1%(n=6).The optimized pretreatment method has the advantages of simpler operation,better reproducibility,better recovery rate,higher detection efficiency and lower detection cost.
作者
邢海燕
汪安
朱志祥
程桂林
黎睿
胡金玲
孙丽婷
XING Haiyan;WANG An;ZHU Zhixiang;CHENG Guilin;LI Rui;HU Jinling;SUN Liting(Chizhou Institute of Quality Supervision and Inspection,Chizhou 247000,China)
出处
《现代食品》
2023年第21期173-177,共5页
Modern Food
基金
2022年安徽省市场监管局科技计划项目“九蒸九晒黄精过程中氨基酸变化规律研究”(2022MK036)。
关键词
高效液相色谱串联质谱法
九华黄精
农药残留
QUECHERS
high performance liquid chromatography-tandem mass spectrometry
jiuhua Polygonatum cyrtonema
pesticide residues
QuEChERS