利用UPLC-MS/MS快速测定大米中8种农药残留  

Rapid determination of 8 pesticide residues in rice by ultra high performance liquid chromatography tandem mass spectrometry

作　　者：张可君[1] 杨皓[2] 张媛[1] ZHANG Ke-jun;YANG Hao;ZHANG Yuan(Tianjin Vocational College of Bioengineering,tianjin 300462,China;Institute of Plant Protection,Liaoning Academy of Agricultural Sciences,Shenyang 110000,China)

机构地区：[1]天津生物工程职业技术学院,天津300462 [2]辽宁省农业科学院植物保护研究所,辽宁沈阳110000

出　　处：《粮食与饲料工业》2023年第6期55-59,共5页Cereal & Feed Industry

摘　　要：基于超高效液相色谱-串联质谱法(UPLC-MS/MS)原理,建立对大米中8种农药残留的快速检测方法。该方法具体工艺流程为:大米样品加水润湿,乙腈和QuEChERS萃取盐包提取稀释,PSA/C18净化管净化分离,再通过电子喷雾正离子(ESI)源,DMRM正离子扫描模式进行检测。结果表明,大米中的8种农药残留在0.1~20 ng/mL范围内线性关系良好,相关系数在0.9994及以上,加标回收率为89.5%~115.8%,相对标准偏差为1.2%~6.9%;7种农药的定量限为1μg/kg,1种农药定量限为2μg/kg,同时,这8种农药的检出限均不超过0.4μg/kg。该检测方法简单、便捷、成本低,准确度和精密度良好,符合GB 2763—2021中的相关标准要求,可以用于日常大米农药残留检测。A rapid detection technique for 8 pesticide residues in rice was studied based on ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The specific process flow of this detection method was as follows:added water to wet rice samples,extracted and diluted with acetonitrile and QuEChERS extraction salt package,purified and separated with PSA/C 18 purification tube,and then detected with electronic spray positive ion(ESI)source and DMRM positive ion scanning mode.The results showed that there was a good linear relationship between the 8 pesticide residues in rice within the range of 0.1-20 ng/mL,with a correlation coefficient of 0.9994 or above.The spiked recovery rate was 89.5%-115.8%,and the relative standard deviation was 1.2%-6.9%.The limit of quantification for 7 pesticides was 1μg/kg,and the limit of quantification for 1 pesticide was 2μg/kg.Meanwhile,the detection limit of these 8 pesticides did not exceed 0.4μg/kg.This detection method is simple,convenient,low-cost,with good accuracy and precision,and meets the relevant standards in GB 2763—2021,and can be used for daily pesticide residue detection in rice.

关 键 词：超高效液相色谱-串联质谱法 大米 农药残留 定量限 检出限 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.6[轻工技术与工程—食品科学与工程] O657.7[理学—分析化学]