气相色谱-质谱法测定甘蔗中除草剂残留量
GC-MS Determination of Residual Amounts of Herbicides in Sugarcane
摘 要
提出了采用QuEChERS法提取净化,气相色谱-质谱法同时测定甘蔗中除草剂莠去津、乙草胺和莠灭净的残留量。采用DB-5MS毛细管柱分离,电子轰击离子源选择离子检测模式进行质谱测定。莠去津、乙草胺和莠灭净的检出限(3S/N)分别为0.001,0.002,0.001 mg·kg-1。在3个浓度水平上对方法的回收率作了测定,测得回收率在88.0%~108.0%,相对标准偏差(n=6)在1.1%~6.9%之间。
QuEChERS
甘蔗
莠去津
乙草胺
莠灭净
GC-MS
QuEChERS
Sugarcane
Atrazine
Acetochlor
Ametryn
Abstract
Three herbicides, i.e., atrazine, acetochlor and ametryn, in sugarcane were extracted and purified by the QuEChERS method, and the contents of the 3 herbicides were determined by GC-MS. The DB-5MS capillary chromatographic column was used for separation, and the electron impact ionization source with selected ion monitoring (SIM) was adopted in MS. Values of detection limit (3S/N) found were 0.001 mg·kg-1 for atrazine, 0.002 mg·kg-1 for acetochlor, and 0.001 mg·kg-1 for ametryn. Recovery was tested at 3 different concentration levels and values of recovery found were in the range from 88.0% to 108.0% with RSD′s (n=6) in the range from 1.1% to 6.9%.
中图分类号 O657.63
所属栏目
基金项目 广西甘蔗研究所基本科研业务专项(G2008011);广西农科院基本科研业务专项(201032)
收稿日期 2011/6/1
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备注王天顺(1980-),男,河南项城人,助理研究员,硕士,主要从事农产品理化性质检验及农药残留安全检测研究。
引用该论文: WANG Tian-shun,YANG Yu-xia,FAN Ye-geng,FANG Feng-xue,MO Lei-xing,LIANG Jun,LIAO Jie,YA Yu. GC-MS Determination of Residual Amounts of Herbicides in Sugarcane[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(11): 1266～1268
王天顺,杨玉霞,范业赓,方锋学,莫磊兴,梁俊,廖洁,牙禹. 气相色谱-质谱法测定甘蔗中除草剂残留量[J]. 理化检验－化学分册, 2011, 47(11): 1266～1268
被引情况:
【1】马健生,王鑫,李丽君,王海娇,肖刚,胡建飞, "固相萃取-气相色谱-质谱法测定土壤中阿特拉津",理化检验－化学分册 51, 79-81(2015)
【2】金党琴,周祥祥,陈庆娣,厉柏嘉, "多壁碳纳米管-十二烷基磺酸钠修饰玻碳电极测定乙草胺",理化检验－化学分册 52, 56-60(2016)
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参考文献
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【2】杨梅,林忠胜,姚子伟,等.气相色谱-质谱联用检测环境水体中的三嗪类除草剂［J］.现代农药, 2007,6(1):23-26．
【3】董振霖,杨春光,肖珊珊,等.气相色谱和气相色谱-质谱法测定食品中乙草胺残留［J］.分析化学, 2009,37(5):698-702．
【4】周瑶敏,熊艳,袁林峰,等.分散固相萃取法快速测定大米中的酰胺类除草剂［J］.中国粮油学报, 2010,25(8):113-116．
【5】李竺,陈玲,郜洪文,等.固相萃取-高效液相色谱法测定环境水样中的三嗪类化合物［J］.色谱, 2006,24(3):267-270．
【6】MELO L F C, COLLINS C H, JARDIM C S F. High-performance liquid chromatographic determination of pesticides in tomatoes using laboratory-made NH2 and C18 solid-phase extraction materials［J］. Journal of Chromatography A, 2005,1073:75-81．
【7】BALDUINI L, MATOGA M, CAVALLI E, et al. Triazinic herbicide determination by gas chromatography-mass spectrometry in breast milk［J］. Journal of Chromatography B, 2003,794:389-395．
【8】LEHOTAY S, MATOVSK K, YUN S J. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes［J］. Journal of Aoac International, 2005,88:630-638．
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