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摘要：建立了气相色谱质谱联用法测定肥料中三十烷醇（TA)和2,4-D的分析方法。主要分为样品的前处理过程和GC/MS分析过程。TA和2,4-D分别以丙酮正己烷（1:1）混合溶液和酸性乙腈为提取剂，并通过超声波辅助萃取，但是由于2,4-D极性较大还需要进行衍生化处理后用于GC/MS分析。实验以8种市售肥料为研究对象，包括有机肥、水溶肥、缓释肥以及腐植肥料等，2,4-D的实验加标回收率为41%-78%，RSD为1.8%，线性范围为1ug/mL-80ug/mL，检出限(S/N≥3)0.06ppm，定量限(S/N≥10)0.2ppm，三十烷醇标样检出限(S/N≥3) 0.001 ppm ，定量限(S/N≥10)0.005ppm,RSD为1.0%，线性范围为0.05ug/mL -80ug/mL实验结果表明，该方法具有灵敏度高，方便快捷等特性，至少可以满足肥料中2,4-D的分析检测要求。35948
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毕业论文关键词：肥料；植物激素；气相色谱质谱联用法；2,4-D；三十烷醇
The analysis of 2,4-D and Triacontanol in the fertilizers
Abstract: The GC/MS method for analysising the growth regulator triacontanol and 2,4-D was developed .This paper can be pided into sample pre-treatment process and GC/MS analysis. Respectively, acetone hexane (1: 1) mixed solution and an acidic acetonitrile as the extraction agent, ultrasonic assisted extraction, but as the 2,4-D has a strong polar ,it should be derivatized before GC /MS analysis. There are eight commercial fertilizer for the study, including organic fertilizer, water soluble fertilizer, slow release fertilizer and humic fertilizers.The recoveries of 2,4-D are 41% -78%, the RSD is 1.8%;the linear ralationship is the range of 1ug / mL-80ug / mL, the detection limit (S/N≥3) is 0.06ppm, the limit of quantification (S/N≥10)is 0.2ppm, triacontanol standard detection limit (S/N≥3 )is 0.001ppm, the limit of quantification (S /N≥10) is 0.005ppm,the RSD is 1.0%, the linear ralationship is range of 0.05ug/mL- 80 ug/mL .The experimental results show that this method has high sensitivity, convenience and so on, it can meet the requires of analisising the 2,4-D from the fertilizer .
KeyWords：Fertilizer;Growth regulator;GC/MS;2,4-D;Triacontanol
目录
1 前言 1
1.1 选题意义 1
1.2 气相色谱-质谱联用仪概要 1
1.2.1 气相色谱原理 2
1.2.2 质谱原理 2
1.2.3 仪器特点 2
1.2.4 应用范围 2
1.3 文献综述 2
1.3.1 肥料成分分析及前处理 3
1.3.2 三十烷醇的分析 5
1.3.3 2,4-D的分析 6
2 实验部分 8
2.1 仪器 9
2.1.1 GCMS仪器参数（2,4-D) 9
2.1.2 GCMS仪器参数（三十烷醇) 10
2.2 标准试剂及用品 10
2.2.1 肥料来源与性状 11
2.3 实验步骤 12
2.3.1 溶剂的配制 12
2.3.2 肥料中2,4-D的分析 12
2.3.3 肥料中三十烷醇的分析 12
2.4 GC/MS仪器操作流程 13
2.4.1 开机顺序 13
2.4.2 进入系统及检查系统配置 13
2.4.3 启动真空泵 13
2.4.4 调谐方法 13
2.4.5 方法编辑 14
2.4.6 样品测定操作 14
2.4.7 后处理操作 14
2.4.8 关机 14
3 结果与讨论 15
3.1 2,4-D结果与讨论 15
3.1.1 提取方案 15
3.1.2 提取剂的选择 15
3.1.3 衍生化反应 15
3.1.4 仪器条件的选择 16