摘要
建立了固相萃取-高效液相色谱-串联质谱法同时测定小麦中双唑草酮和环吡氟草酮残留的方法。小麦样品中双唑草酮和环吡氟草酮采用酸化乙腈提取,氯化钠和无水硫酸镁盐析,HLB固相萃取柱净化,以0.1%甲酸水-0.1%甲酸乙腈为流动相梯度洗脱,ACQUITY UPLC BEH C18色谱柱分离,在电喷雾离子源正模式下,采用多反应监测(MRM)模式测定,基质匹配标准曲线外标法定量。结果表明,双唑草酮和环吡氟草酮在2~100μg·L^(-1)范围内线性关系良好,相关系数均大于0.998;检出限为2μg·kg^(-1),定量限为6μg·kg^(-1)。在6、20、50μg·kg^(-1)添加水平下,双唑草酮的平均回收率为93.9%~99.6%,相对标准偏差(RSD)为2.2%~4.8%,环吡氟草酮的平均回收率为83.6%~90.7%,相对标准偏差为1.4%~4.5%(n=6)。该方法灵敏、准确,适用于小麦中双唑草酮和环吡氟草酮残留的测定。
A method was established for the simultaneous determination of bipyrazone and cypyrafluone in wheat by solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry.Bipyrazone and cypyrafluone in wheat samples were extracted by acidified acetonitrile,salted out by sodium chloride and anhydrous magnesium sulfate,cleaned up by HLB solid phase extraction column,separated by ACQUITY UPLC BEH C18 column with gradient elution of water(containing 0.1%formic acid)and acetonitrile(containing 0.1%formic acid)as the mobile phase,detected by positive electrospray ionization using multiple reaction monitoring(MRM)mode and finally quantified by external standard method of matrix calibration curve.Good linear relationship displays in the concentration range of 2-100μg·L^(-1)for bipyrazone and cypyrafluone with correlation coefficient(r)greater than 0.998.The limits of detection of them are 2μg·kg^(-1),and the limits of quantitation are 6μg·kg^(-1).At three spiked concentration levels of 6,20 and 50μg·kg^(-1),the average recoveries of bipyrazone are 93.9%-99.6%,with relative standard deviations(RSDs)of 2.2%-4.8%,and the average recoveries of cypyrafluone are 83.6%-90.7%,with RSDs of 1.4%-4.5%(n=6).The method is sensitive,accurate and suitable for determination of bipyrazone and cypyrafluone in wheat.
作者
董睿男
边海涛
勇艳华
李鹏
苏春敏
刘杨
DONG Ruinan;BIAN Haitao;YONG Yanhua;LI Peng;SU Chunmin;LIU Yang(Dalian Center for Certification and Food and Drug Control,Technology Innovation Center of Food Safety Technique of Inspection for State Market Regulation(Rapid Screening and Traceability for Edible Agricultural Product Safety),Dalian 116630,Liaoning)
出处
《浙江农业科学》
2024年第12期3010-3014,共5页
Journal of Zhejiang Agricultural Sciences
基金
国家市场监督管理总局科技计划项目(2020MK114)。
关键词
固相萃取
高效液相色谱-串联质谱
双唑草酮
环吡氟草酮
小麦
solid-phase extraction
high performance liquid chromatography-tandem mass spectrometry
bipyrazone
cypyrafluone
wheat
