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高效液相色谱-质谱法测定谷物中11种三嗪类农药残留

High Performance Liquid Chromatography/Mass Spectrometry Method for Determination of Grain of 11 Kinds of Triazine Pesticide Residues

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【作者】 海华胡婕李光浩

【Author】 HAI Huaa,HU Jiea,LI Guang-haob(a.Department of Life Sscience;b.Modern Educational Technology Center,Dalian Nationalities University,Dalian Liaoning 116605,China)

【机构】 大连民族学院生命科学学院大连民族学院现代教育中心

【摘要】 建立了高效液相色谱-紫外检测-质谱定性法,用于谷物中11种三嗪除草剂(西玛津、阿特拉津、扑灭通、特丁通、莠灭净、扑灭津、特丁津、扑草净、扑莠净、草达津、杀草净)残留量的同时测定。样品经丙酮提取,SCX固相萃取柱净化,用高效液相色谱-紫外检测-质谱法测定,液相外标法定量。对样品前处理和色谱分离条件进行了研究和优化。11种三嗪类除草剂在0.02×10-6~1.0×10-6g.mL-1范围内线性良好,相关系数为0.998 7~0.999 9,在0.02~1.0μg.g-1质量浓度范围内,平均加标回收率在61.6%~111.0%,相对标准偏差为2.4%~6.1%。方法简便、快速,净化效果较好,可同时满足进、出口谷物中多种除草剂残留量的检验要求。

【Abstract】 A high performance liquid chromatography-UVdetection-mass spectrometry qualitative method has been developed for determination of residues 11 triazine herbicides(simazine,atrazine,prometon,terbumeton,ametryne,propazine,terbuthylazine,prometryne,terbutryne,trietazine,dipropetrne) in grain.Triazine herbicides were extracted from grain with acetone and cleaned up with SCX solid phase extraction cartridges.Then triazine herbicides extracted were analyzed by HPLC with ultraviolet and mass spectrometric detection.The pretreatment method of sample and chromatographic conditions of analysis were optimized.The linear range for the 11 kinds of triazine herbicides were 0.02 × 10-6 ~ 1.0 × 10-6g·mL-1,with correlation coefficient of 0.9987 ~ 0.9999.The average recovery rate for the 11 triazine in spiked grain were in the range of 61.6 % ~ 111.0 %,and relative standard deviation were between 2.4 % and 6.1 %.The method is simple,rapid,and has a better purification effect,which can meet the requirement for determination of herbicide residues in grain.

【关键词】 三嗪农药谷物液相色谱-质谱固相萃取
【Key words】 triazinic herbicidesgrainsHPLC-MSSPE
  • 【文献出处】 大连民族学院学报 ,Journal of Dalian Nationalities University , 编辑部邮箱 ,2011年01期
  • 【分类号】TS210.7
  • 【被引频次】2
  • 【下载频次】371
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