摘要
建立了QuEChERS结合高效液相色谱-串联质谱法(HPLC-MS/MS)同时检测植物源食品(卷心菜、苹果、柑橘、香菇、葡萄干、玉米、大米、小麦、大麦)中Tolpyralate和环哒嗪草酯两种新型除草剂的检测方法。样品用乙腈提取,经改良QuEChERS粉末净化,GL Sciences InertSustain C18色谱柱(150 mm×2.1 mm,3μm)分离,用HPLC-MS/MS多反应离子监测扫描模式(Multiple reaction monitoring,MRM)进行检测,基质匹配溶液外标法定量。结果表明:两种除草剂在0.5~20.0 ng/mL范围内线性关系良好(R^(2)>0.9914),检出限(S/N=3)为0.14~0.90μg/kg,定量限(S/N=10)为0.47~3.00μg/kg,回收率为65.4%~111.2%(RSD≤10.2%,n=6),满足日本、美国、加拿大制定的农药残留限量标准。该方法操作简单、灵敏度高,适用于多种植物源性食品中Tolpyralate和环哒嗪草酯的快速筛查、定性与定量分析。
In this study,a QuEChERS method coupled with high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was developed for the simultaneous determination of two new herbicides,tolpyralate and cyclopyrimorate,in food of plant origin(cabbage,apples,mandarin oranges,shiitake mushrooms,sultanas,maize,rice,wheat and barley).The sample was extracted with acetonitrile,cleaned up by modified QuEChERS powder,separated on a GL Sciences InertSustain C18 column(2.1 mm×150 mm,3μm),and then analyzed by LC-MS/MS with multiple reaction monitoring(MRM)scan mode and quantified by matrix-matched external calibration method.The results demonstrated that the linearity of the two herbicides was satisfactory within the range of 0.5-20 ng/mL(R^(2)>0.9914).The limits of detection(S/N=3)ranged from 0.14 to 0.90μg/kg,while the limits of quantification(S/N=10)ranged from 0.47 to 3.00μg/kg.The recoveries were within the range of 65.4%to 111.2%(RSD≤10.2%).The determined results met the pesticide residue limits set by Japan,the US,and Canada.The method is straightforward,highly sensitive,and suitable for the rapid screening,qualitative,and quantitative analysis of tolpyralate and cyclopyrimorate in a wide range of plant-derived foods.
作者
孙千然
苟圆
刘俊
粟有志
SUN Qianran;GOU Yuan;LIU Jun;SU Youzhi(Chengdu Customs Technology Center,Chengdu 610041;Yining Customs Technology Center,Yining 835000)
出处
《分析科学学报》
北大核心
2025年第4期415-422,共8页
Journal of Analytical Science
基金
四川省科技创新人才项目(2023JDRC0007)。
关键词
QUECHERS
高效液相色谱-串联质谱
植物源食品
多基质
新型除草剂
QuEChERS
High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
Plant-derived foods
Multi-matrix
Novel herbicides
