摘要：本实验采用三级四级杆液质联用仪，建立并优化了马铃薯和土壤中烯草酮的残留分析的方法。经优化后的方法为:在锥形瓶中称取样品5.00 g，加入20.0 mL超纯水，2.0 mL乙酸铅，加入20.0 mL乙腈，在摇床上摇晃2 h后抽滤，盐析，静置分层。取上层清液1 mL，用30 mgC18分散固相萃取填料进行净化，净化后的溶液用0.22 μm微孔滤膜过滤，装入进样小瓶上机。流动相为乙腈-水-甲酸(体积比60∶40∶0.1)，流速0.3 mL/min；柱温为35 ℃；进样量4 μL。离子对360.1/164.1为定量离子，对烯草酮残留进行定量分析。实验进行了三个添加水平测试，分别为0.05 mg•kg-1、0.1 mg•kg-1和0.2 mg•kg-1，得到的平均回收率为85.3%~86.8%，相对平均偏差（RSD）小于5%。烯草酮在马铃薯上的最大残留限量为0.1 mg•kg-1，该方法的检出限为0.010 mg•kg-1，定量限为0.020 mg•kg-1，该方法的准确性、精确性以及灵敏度符合农药残留分析测定的要求。8930
关键字：烯草酮，残留分析，液质联用，马铃薯
Distribution of Clethodim in potato and soil
Abstract:In this study,we use the three quadrupole LC-MS instrument,the analysis method of clethodim residues in potato and soil is established and optimized.The method after optimization is: weigh 5.00 g sample in the conical flask,add 20.0 mL ultrapure water,2.0 mL lead acetate,20.0 mL acetonitrile, shaking 2 h in a shaker,filtration, salting rested,stratification.Take the supernatant fluid 1 mL,With 30 mgC18 dispersive solid-phase extraction packing for purificatio,after purification, the solution with 0.22 um microporous membrane filter, load the sample vial and Ready to machine.Mobile phase is acetonitrile - water - formic acid (volume ratio 60:40:0.1), the flow rate of 0.3 mL/min; Column temperature of 35 ℃; Sample quantity 4 uL.Ion on 360.1/164.1 is quantitative ion,ion pair 360.1/164.1 as a quantitative ion,analysis residues of clethodim.Experiment was carried out three add level test,respectively are 0.05 mg•kg-1,0.1 mg•kg-1,0.2 mg•kg-1.The average recovery was 85.3% ~ 85.3%, average relative deviation (RSD) is less than 5%.The method detection limit is 0.010 mg•kg-1, quantitative limit is 0.020 mg•kg-1, accuracy, precision and sensitivity of this method meets the requirement of pesticide residue analysis determination.
Keywords: Clethodim, residue analysis, LC-MS, potato

目录
1  前言
1.1烯草酮的理化性质..1
1.2烯草酮的生物活性..1
1.3烯草酮的环境影响与动物毒性1
1.4 烯草酮的残留分析方法..2
1.4.1 液相色谱串联质谱法分析..2
1.4.2 近红外光谱法分析..3
1.4.3核磁共振氢谱法分析..3
1.5烯草酮的最大残限度.4
1.6 立题依据..5
2  实验部分
2.1 主要的试剂和仪器设备6
2.1.1 试剂与材料.6
2.1.2 仪器设备..6
2.2 分析步骤6
2.2.1 提取.6
2.2.2 净化.7
2.2.3 测定.7
2.2.3.1 仪器条件.7
2.2.3.2 结果的计算和表达7
2.3标准曲线与检出限度..8
  2.3.1标准曲线8
  2.3.2检出限与定量限9
3  烯草酮残留分析方法的优化
3.1提取剂对于回收率的影响11
3.2提取方式对于回收率的影响..11
3.3提取剂量对于回收率的影响..12
3.4加水对于回收率的影响.13
3.5加水量对于回收率的影响13
3.6氨基柱和Florisil柱对于回收率的影响14
3.7分散固相萃取填料对标准品的吸附15
3.8C18量对于回收率的影响.15
3.9添加乙酸铅对于回收率的影响..16
4  结论
4.1对马铃薯和土壤样品进行添加回收实验.18
4.2不同添加量的添加回收..19
5  总结..20
6  致谢..21
参考文献22
  烯草酮在马铃薯和土壤上分布研究:http://www.youerw.com/shengwu/lunwen_7469.html