摘要：本文采用液质联用仪，优化并建立了检测小麦中扑草净残留含量的分析检测方法。样品通过乙腈震荡提取，在经过优化后的QuEChERS方法净化后，采用Aglilent EC-C18色谱柱为分离柱，以5mmol乙酸胺和甲醇为流动相，梯度洗脱，LC-MS/MS电喷雾正离子模式下分析测定。实验进行三个添加水平，为0.01mg/kg、0.05mg/kg和0.1mg/kg，得到平均添加回收率为86.1%-89.6%，相对标准偏差为1.4%-2.6%。液相色谱质谱联用仪法检测扑草净的线性范围为0.02-0.2μg/ml，相关系数为r2=0.9994。方法的检出限为0.1μg/kg。结果表明，该方法具有检出限低、灵敏度高、快速、前处理方法简单、回收率高等优点，适用于小麦中扑草净的残留检测分析。8761
关键词: 扑草净；小麦；农药残留；液相色谱质谱联用仪
Determination of residual prometryn in wheat
Abstract: This article uses the liquid chromatography mass spectrometry to develop and optimize the analysis detection method in residues of prometryn on wheat. Sample was extracted by acetonitrile, and the method QuEChERS has been validated for the extraction. The compound was separated on an Aglilent EC-C18 column（2.1×100mm，2.7μm）with 5mmol/L ammonium acetate and methanol as mobile phase under gradient elution．The extract was measured directly by LC- MS/MS with electrospray ionization in negative mode. The experiments are carried out three add proficiency tests, which are 0.01mg/kg, 0.05mg/kg and 0.1mg/kg. The average recovery is 86.1%-89.6%, and the relative standard deviation is 1.4%-2.6%. The liquid chromatography mass spectrometry detect that the linear range of the prometryne is 0.02-0.2μg/ml and the correlation coefficient of r2 = 0.9988. The detection limits of the method was1.0μg/kg. This method is sensitive and quick, and has low detection limit, high recovery range, and simple sample pre-treatment method. This method could be used to determine residual metolachlor in wheat.
Keywords: prometryn; wheat; pesticide residue analysis; chromatography mass spectrometry (LC-MS/MS)
目 录
1引言 1
1.1 农药的发展史 1
1.2 三嗪类除草剂对小麦的使用情况 1
1.3 农药残留检测技术的发展 2
1.4 扑草净的理化性质 3
1.5 扑草净常用的残留检测方法 3
1.5.1 气象色谱法 3
1.5.2 气象色谱质谱联用仪法 4
1.5.3 高效液相色谱法 5
1.6 扑草净的动物与植物活性 6
1.7 扑草净的生物活性 7
1.8 扑草净在不同国家的限量 7
1.9 本文主要研究内容及意义 8
1.9.1 研究内容 8
1.9.2 研究意义 8
2 实验部分 10
2.1 实验试剂与设备 10
2.1.1 实验试剂 10
2.1.2 实验设备 10
2.2 实验材料 11
2.3 分析步骤 11
2.3.1 提取 11
2.3.2 净化 11
2.3.3 测定 11
3 结果与讨论 14
3.1 仪器条件的优化 14
3.1.1 流动相的选择 14
3.1.2 质谱条件的选择 14
3.2 提取溶剂的选择 14
3.2.1 提取溶剂的选择 14
3.2.2 提取溶剂量的选择 15
3.2.3 提取过程中加水量对扑草净回收率的影响 15
3.2.4 提取方式的比较 16
3.3 吸附剂的选择 17
3.3.1 不同种类吸附剂对扑草净回收率的影响 17 小麦残留扑草净的测定+文献综述:http://www.751com.cn/shiping/lunwen_7211.html