多壁碳纳米管分散固相萃取-液质联用技术测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留量.pdf

第5卷第4期
食品安全质量检测学报
VOL 5 No 4
2014年4月
Journal of Food Salcly and Quality
Apr.,2014
多壁碳纳米管分散固相萃取-液质联用技术测定
茶叶中草甘滕、草铵滕、氨甲基酸残留量
冯月超,马立利,贾丽,张春梅,刘艳",范筱京,潘灿平2
(1.北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心,北京100089
2.中国农业大学理学院,北京100193)
摘要:目的建立茶叶中草甘膦、草铵膦和氨甲基膦酸残留量的超高效液相色谱串联质谱分析方法。方法
样品经水提取后采用分散固相萃取技术,以多壁碳纳米管( MWCNTS)和N丙基乙二胺鍵合固相吸附剂(PSA)吸
附提取液中的杂质,上清液用9-芴基氯甲酸酯IMOC-C衍生。衍生物用 BEII C1s进行分离,以乙腈-4mmo
乙酸铵水溶液为流动相,电喷雾正离子模式电离(IST).多反应监测模式检測(MRM),外标法定量。结果方
法的线性范围是0.1~1ugml,相关系数大于0.990,定量限为10gkg.以绿茶为基质,三种物质添加水平分
别为0.25、0.50、1.00mg/kg.回收率范围分别为草甘隣95%6~-116%、草铵98%0-118%、,氨甲基膦酸749%-849%,
精密度均小于6.79%0=6)。结论该方法具有简便快速、灵敏度高、准确性强等特点,适合于测定茶叶中草甘
、草铵螣和氨甲基膦酸的含量
关键词:液质联用;草甘膦;草铵滕;氨甲基磷酸;茶叶;多壁碳纳米管;分散固相萃取
Determination of glyphosate, glufosinate and aminomethylphonic acid
residues in tea by liquid chromatography-tandem mass spectrometry
using multi-walled carbon nanotubes as dispersive solid-phase
extraction sorbent
FENG Yue-chao, MA Li-li JIA Li, ZHANG Chun-mei, LIU Yan, FAN Xiao-jing, PAN Can-ping
(1. Beiiing Engineering Research Center of Food Safety/sis, Beijing Center for Physical and Chemical nalysis
Beijing 100089, China; 2. College of Science, China Agricultral tniwersity, Beijing 100193, China)
ABSTRACT: Objective An ultra performance liquid chromatography-landem mass spectrometry(uplc-ms/MS)
analysis mcthod was established for simultancous determination of glyphosate, glufosinate and aminomethyl-
phonic acid (AMP/ )in tea. Methods The sample was extracted with watcr, and cleaned up by multi-wallcd
carbon nanotubes(MW CNTS)and primary-sccondary amine(PS A)as dispersive solid-phasc cxtraction sorbent
then derived using fluorenyl methyl chloroformate(pmoc-c1). The derivatives wcrc scparated by ACQUTTY
UPI. C BI: I Cs column, using acetonitrile and 4 mmol/. ammonium acetate as the mobile phase. The identiti
cation and quantification of glyphosate, glufosinate and AMPA were carricd out by MS/MS in positive clectro-
基金项目:北京市财政资金创新工程项目(PXM20131783050000
Iund: Supported by Beijing I'inancial Iound Project on Creative I ineering Project(PXM2013178305000004
通讯作者:刘艳,博士,副研究员,主要研究方向为食品安全检測技术。T:-mai:xgly36163.c0m
Corresponding author: LIU Yan, Rcscarch Associate, Bcijing cntcr for Physical and Chcmical Analysis, No 27, West Third Ring Road, Hai
dianDistrict,Beijing100089,china.e-mail:xply36(a163.com