分散固相萃取∕衍生化-高效液相色谱-串联质谱法同时测定水和食品中草甘膦、草铵膦和氨甲基膦酸残留.pdf

第8卷第4期
食品安全质量检测学报
2017年4月
Journal of Food Safety and Quality
Apr.,2017
分散固相萃取衍生化-高效液相色谱串联质谱法
同时测定水和食品中草甘膦、草铵膦和
氨甲基膦酸残留
张燕’,舒平,陆敏,甘献明,赵用,李颖
(大理州质量技术监督综合检測中心,大理671000)
摘要:目的建立高效液相色谱-串联质谱法测定水和食品中草甘膦、草铵膦和氨甲基膦酸的残留量。方法
样品经纯水涡旋超声提取,二氯甲烷去除脂肪,C18分散固相萃取净化,(水样)净化液在硼酸盐缓冲液中加入9-
芴基甲基三氯甲烷(FMOC-CD)丙酮溶液进行衍生化2h以上,经0.22m微孔滤膜过滤,经 CAPCELLCORE
C1g柱分离,用5 mmol/L乙酸铵溶液和乙腈为流动相梯度洗脱,采用电喷雾负离子多反应监测模式检测,外标
法定量。结果草甘膦、草铵膦和氨甲基膦酸在0.5~40μg/L浓度范围内呈良好的线性关系(r>0.999,方法
定量限为0.5pgkg。在0.5、5.0和20Hg/kg添加水平时,平均回收率为70.1%~104.19%,相对标准偏差为
0.6%6-89%(m=6)。结论该方法分析速度快,净化效果好,杂质干扰小,回收率高,重复性好,适用于水和食
品中草甘、草铵膦和氨甲基氨酸留量的测定
关键词:分散固相萃取;草甘膦;草铵膦;氨甲基膦酸;衍生化;高效液相色谱-串联质谱法
Simultaneous determination of glyphosate, glufosinate and aminomethy
residues in water and foods by dispersive solid phase extraction
derivatization-high performance liquid chromatography-tandem
mass spectrometry
ZHANG Yan, SHU Ping, LU Min, GAN Xian-ming, ZHAO Yong, LI Ying
(Dali State Comprehensive Technical Inspection Center, Dali 671000, China)
ABSTRACT: Objective To establish a method for determination of glyphosate, glufosinate and aminomethyl
residues in water and foods by high performance liquid chromatography-tandem mass spectrometry(hplc-ms/MS
Methods The samples were extracted by pure water vortex with ultrasound, and defatted with dichloromethane
then purified by Cg dispersive solid phase extraction column. Purified liquid(water)was adjusted PH by phosphate
saline buffer and added 9-fluorene methyl chloroform(fmoc-ci)acetone solution for derivatization for 2 h at least
Derived compounds were filtered through 0.22 um millipore membrane. The sample extract was separated b
CAPCELLCORE Cl column with 5 mmol/L ammonium acetate-acetronitrile as mobile phase for gradient elution,
and then identified by electrospray ionization(ES1)in negative mode and multiple reaction monitoring mode, and
基金项目:云南省质量技术监督局科技计划项目(20I7 ynzgkj05)
Fund: Supported by Science and Technology Project of Yunnan Provincial Bureau of Quality and Technical Supervision(2017ynzjkj05
通讯作者:张燕,高级工程师、主要研究方向为食品安全检测。E-mail:shiyan230@163.com
Corresponding author: ZHANG Yan, Senior Engineer Dali State Comprehensive Techical Inspection Center, Economic Development Zone 1 Box
Dali67100,ChinaE-mail:shiyan1230@163.com
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