摘要
建立了一种超高液相色谱-串联质谱法直接测定食品中草甘膦及其代谢物氨甲基膦酸的方法。样品用水提取,固相萃取小柱(HLB)净化,以5 mmol/L的乙酸铵溶液和乙腈为流动相,梯度洗脱,氨基柱色谱分离,采用电喷雾离子源、负离子扫描模式和多反应监测模式测定。草甘膦和氨甲基膦酸的线性范围分别是5.00~100μg/L和10.0~200μg/L,相关系数(R2)均大于0.995。方法的检出限分别为10.0和20.0μg/kg,定量限分别为25.0和50.0μg/kg。草甘膦和氨甲基膦酸在3个加标水平(25.0, 50.0和250μg/kg;50.0, 100和500μg/kg)下的回收率为72.1%~90.7%,相对标准偏差(RSD, n=6)为5.49%~9.01%。该方法简便、快捷、有效,前处理简单,样品无需衍生,结果稳定性高,可满足各类食品的检测需求。
A method for determination of glyphosate and aminomethyl phosphonic acid in food by ultra high performance liquid chromatography triple quadrupole mass spectrometry(UPLC-MS/MS) was established. General samples were extracted by water and were purified by solid phase extraction column(HLB). Ammonium acetate solution of 5 mmol/L and acetonitrile were used as mobile phase. Gradient elution and amino column chromatography were used for separation. Electrospray ion source, negative ion scanning mode and multi-reaction monitoring mode were used for mass spectrometry detection. The linear ranges of glyphosate and aminomethyl phosphonic acid were 5.00-100 μg/L and 10.0-200 μg/L, respectively, and the correlation coefficient(R2) was greater than 0.995. The detection limits of the method were 10.0 and 20.0 μg/kg, and the quantitative limits were 25 and 50 μg/kg, respectively. The recoveries of glyphosate and aminomethyl phosphonic acid at the three standard levels(25.0, 50.0 and 250 μg/kg;50.0, 100 and 500 μg/kg) were 72.1%-90.7%, and the relative standard deviation(RSD, n=6) was 5.49%-9.01%. The method had the advantages of simple pretreatment, no derivation of samples, high stability, simpleness, speediness and effective results, and it could meet the testing requirements of all kinds of food.
作者
孙文闪
章虎
张安平
诸骏杰
余鹏飞
沈雄雅
SUN Wenshan;ZHANG Hu;ZHANG Anping;ZHU Junjie;YU Pengfei;SHEN Xiongya(Greentown Agricultural Testing Technology Co.,Ltd.,Hangzhou 310051;College of Environment,Zhejiang University of Technology,Hangzhou 310014)
出处
《食品工业》
CAS
北大核心
2020年第5期324-328,共5页
The Food Industry
基金
国家重点研发计划资助(2018YFC1602800)。
关键词
超高液相色谱串联质谱
草甘膦
氨甲基膦酸
食品
ultra high performance liquid chromatography triple quadrupole mass spectrometry(UPLC-MS/MS)
glyphosate
aminom ethyl phosphonic acid
food
