超高效液相色谱-串联质谱法同时测定红花中甜菜安、甜菜宁及乙氧呋草黄残留的分析方法研究OA
Simultaneous Determination of of Desmedipham,Phenmedipham,and Ethofumesate Residues in Safflower by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
本研究旨在建立一种快速、灵敏、准确的超高效液相色谱-串联质谱(UPLC-MS/MS)方法,用于同时测定鲜红花和干红花中氨基甲酸酯类除草剂甜菜安、甜菜宁以及呋草黄类除草剂乙氧呋草黄的残留量.样品经0.1%甲酸-乙腈溶液提取,氯化钠盐析,取上层有机相过滤后直接进样分析,采用外标法定量.结果表明,甜菜安、甜菜宁及乙氧呋草黄在0.005~0.2 mg/L(溶剂)和0.01~1 mg/L(基质)浓度范围内线性关系良好,相关系数(R)均>0.9970.在0.02、0.1和1mg/kg3个添加水平下,3种目标化合物在鲜红花和干红花中的平均回收率范围为88%~110%,相对标准偏差(RSD)为1.5%~12.3%.方法的定量限均为0.02 mg/kg,最低检出量在10~2 ng水平.基质效应评价显示,鲜红花和干红花对3种目标化合物均存在显著的基质抑制效应,分别为-42.4%至-91.3%.本方法操作简便、重现性好、灵敏度高,完全满足红花中甜菜安、甜菜宁及乙氧呋草黄残留的快速检测与确证分析要求,为相关产品的质量安全监管提供了有效的技术手段.
This study aimed to establish a rapid,sensitive,and accurate method using Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)for the simultaneous determination of the carbamate herbicides desmedipham and phenmedipham,and the benzofuran herbicide ethofumesate in fresh and dried safflower(Carthamus tinctorius L.).The samples were extracted with 0.1%formic acid-acetonitrile solution,followed by liquid-liquid partitioning induced by sodium chloride.The upper organic phase was filtered and directly injected for analysis,and quantification was performed using the external standard method.The results showed that all three analytes exhibited good linearity within the concentration ranges of 0.005~0.2 mg/L(in solvent)and 0.01~1 mg/L(in matrix),with correlation coefficients(R)greater than 0.9970.At fortification levels of 0.02,0.1,and 1 mg/kg,the average recoveries ranged from 88%to 110%,with relative standard deviations(RSDs)of 1.5%and 12.3%.The limits of quantification(LOQs)for all analytes were 0.02 mg/kg,and the limits of detection(LODs)were at the 10-2 ng level.Matrix effect evaluation revealed significant signal suppression in both fresh and dried safflower matrices,ranging from-42.4%to-91.3%.This method is simple,reproducible,and highly sensitive,meeting the requirements for rapid screening and confirmatory analysis of desmedipham,phenmedipham,and ethofumesate residues in safflower,and providing an effective technical tool for quality and safety supervision of related products.
宋广悦;朱丹;滕瑶;陈国峰;魏民
黑龙江省植检植保站,黑龙江 哈尔滨 150036黑龙江省植检植保站,黑龙江 哈尔滨 150036黑龙江省农业科学院农产品质量安全研究所,黑龙江 哈尔滨 150086黑龙江省农业科学院农产品质量安全研究所,黑龙江 哈尔滨 150086黑龙江省植检植保站,黑龙江 哈尔滨 150036
农业科技
红花甜菜安甜菜宁乙氧呋草黄残留分析
safflowerdesmediphamphenmediphamethofumesateresidue analysis
《农药科学与管理》 2026 (7)
34-40,7
评论