搜索
中文摘要I2种未知农药的鉴定与分析摘要采用气相色谱法、红外光谱法、高效液相色谱法、原子吸收光谱法对两种农药未知物进行了定性、定量分析研究。顶空气相色谱-火焰光度检测器（HS-GC-FPD）法证实了未知物1酸解后放出CS2，经红外谱图比较进一步确认其为代森类杀菌剂（EBDCs）。通过原子吸收光谱法测定农药未知物1中Mn和Zn的含量分别为8.67%和2.5%，最后确证了农药未知物1的主要成分为代森锰锌而非代森锰或代森锌。采用红外光谱法测定未知物2，通过解谱和对照标准谱图，初步确定其主要成分为三苯基乙酸锡。通过高效液相色谱法（HPLC），采用紫外检测器、NH2分离柱，以甲醇∶水=80∶20（V/V）为流动相，对农药未知物2进行了定量分析和进一步的确证定性。结果计算得出农药未知物2中三苯基乙酸锡的含量为13.35%，检出限为0.2μg，添加回收试验表明其平均回收率和相对标准偏差分别为100.0%~100.4%，1.96%~1.99%，其准确度和精度均满足常量分析的要求。农药未知物2中Sn的含量为15.4%，进一步确证了农药未知物2的主要成分为三苯基乙酸锡。关键词：未知农药；分析；红外光谱法；高效液相色谱法；原子吸收光谱法ABSTRACTIIDENTIFICATIONANDANALYSISONTWOKINDSOFUNKNOWNPESTICIDESABSTRACTTwokindsofunknownpesticideswerestudiedqualitativelyandquantitativelybyGC,IRandHPLC,aswellasAAS.HeadspaceGC-FPDmethodconfirmedthattheunknownpesticideNo.1re-leasedCS2afterdecomposedbyacid.ThroughcomparingIRspectrumitfurtherconfirmedthatthepesticidewasEBDCs.ThecontentofMnandZninunknownpesticidesNo.1was8.67%and2.5%respectively,determinedbyatomicabsorptionspectrometry.ItfurtheridentifiedthatthemajorcomponentofunknownpesticideNo.1wasMancozeb,ratherthanmaneborzineb.TheunknownpesticideNo.2wasfirstdeterminedbyIR.Throughparsingandreferringtothestandardspectrum,itconfirmedthatthemajorcomponentwasini-tiallytriphenyltinacetate.ThentheunknownpesticideNo.2wasdeterminedbyHPLCwithultravioletphotometricdetector.TheanalyticalcolumnwasAGTNH2,whilethemobilephasewasmethanolandwaterwiththevolumeproportionof80∶20(V/V).TheproportionoftriphenyltinacetateintheunknownpesticideNo.2was13.35%,calculatedusingthemethod.Thedetectionlimitwas0.2μg.Thefortifica-tionamountshowedthattheaveragerecoveryandrelativestandarddeviationwere,respectively,100.03%~100.39%,1.96%~1.99%.Itshowedthattheaccuracyofthismethodandaccuracywouldbothmeettherequirementsofconstantanalysis.ThecontentofSninunknownpesticideNo.2was15.4%,confirmingthemajorcomponentofunknownpesticidesNo.2.KEYWORDS:unknownpesticide;analysis;IR;HPLC;FAAS目录1前言.............................................................................................................................................11.1农药分析概述............................................................................................................................11.1.1农药分析的定义.....................................................................................................................11.1.2农药分析的意义.....................................................................................................................11.1.3农药分析的方法.....................................................................................................................11.2四大定性谱图的概述................................................................................................................21.2.1紫外光谱.................................................................................................................................21.2.2红外光谱.................................................................................................................................31.2.3质谱.........................................................................................................................................31.2.4核磁共振.................................................................................................................................41.2.5四大谱图的比较.....................................................................................................................41.3原子吸收光谱法简介................................................................................................................51.3.1原子吸收光谱仪结构.............................................................................................................51.3.2原子吸收光谱法的原理.........................................................................................................61.3.3原子吸收光谱法的特点及应用.............................................................................................71.42种未知农药的概述..................................................................................................................81.4.1农药未知物1..........................................................................................................................81.4.2农药未知物2..........................................................................................................................92材料与方法.................................................................................................................................132.1气相色谱顶空进样初步确定农药未知物1的类别..............................................................132.1.1仪器及设备...........................................................................................................................132.1.2试剂及耗材...........................................................................................................................132.1.3气相色谱的操作条件...........................................................................................................132.2红光光谱法对2种未知农药定性..........................................................................................132.2.1仪器及设备..........................