GC-ECD法测定中药配方颗粒中20种有机氯农药残留量

Determination of 20 kinds of organochlorine pesticide residues in Chinese dispensing granules by GC-ECD

关键词:  中药配方颗粒  有机氯农药  GC-ECD  Florisil固相萃取  硫酸

Key words:  Chinese dispensing granules  organochlorine pesticide residues  GC-ECD  Florisil solid phase extraction  sulfuric acid

摘要:

本研究在于建立10种中药配方颗粒中20种有机氯农药：六六六（α-BHC、β-BHC、γ-BHC和δ-BHC 4种异构体），滴滴涕（pp'-DDE、pp'-DDD、pp'-DDT和op'-DDT 4种同系物），五氯硝基苯，艾试剂，七氯，环氧七氯，异狄氏剂，狄氏剂，六氯苯，五氯苯胺，五氯甲基苯硫醚，顺氯丹，反氯丹和氧氯丹残留量的GC-ECD测定方法。将配方颗粒样品经乙酸乙酯超声提取，再经Florisil固相萃取小柱及硫酸磺化净化，采用DB-5气相毛细管色谱柱（柱长60 m，内径0.25 mm，膜厚0.25 μm）检测。所使用的方法为程序升温，ECD检测器检测，内标法定量，进样口温度250℃，检测器温度300℃，载气为高纯氮气（99.999%），流速为1.0 mL·min^-1，脉冲不分流进样，进样量为1 μL。结果表明：20种农药成分在2～100 μg/L时有良好的线性关系。20种农药成分加标回收率范围为71.37%～118.06%，相对标准偏差（RSD）为1.19%～7.88%。该方法简便、准确，可应用于中药配方颗粒中20种有机氯农药留量的同时检测。

Abstract:

To establish a GC-ECD method to determine 20 kinds of organochlorine pesticide residues[benzene hexachloride (α-BHC,β-BHC,γ-BHC,δ-BHC),DDT (pp'-DDE,pp'-DDD,pp'-DDT,op'-DDT),PCNB,aldrin,heptachlor,heptachlor epoxide,endrin,dieldrin,hexachlorobenzene,pentachlorophe-nol aniline,methyl-pentachlorophenyl sulfide,cis-chlordane,trans-chlordane,oxy-chlordane] in Chinese dispensing granules.Chinese dispensing granules samples were ultrasonically extracted with ethyl acetate,and the extract was purified through Florisil solid phase extraction (SPE)cartridge,and then treated with sulfuric acid to remove the impurities.GC was performed on DB-5 gas capillary column (the column length 60 m,inner diameter 0.25 mm,thickness of film 0.25 μm) with electron capture detector.The methods used were temperature programming and ECD detector detection.The internal standard method was used for quantitative analysis.The inlet temperature was 250℃ and the detector temperature was 300℃.The carrier gas was high purity nitrogen at a flow rate of 1.0 mL·min^-1.The pulse was not split injection,and the injection volume was 1 μL.The results showed that there were good linear relationships between 20 pesticide components at 2~100 μg/L.The spiked recovery rates of 20 pesticides were in the range of 71.37% to 118.06%,and the relative standard deviation (RSD) was 1.19% to 7.88%.The method is simple and accurate,and can be applied to the simultaneous detection of 20 organochlorine pesticide residues in Chinese dispensing granules.