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中药菊花中12种农药残留量的气相色谱检测方法研究
Determination of 12 pesticide multiresidues in Dendranthema moriflolium by gas chromatography
【摘要】 采用气相色谱仪同时检测中药菊花中12种有机磷和有机氯农药的残留量。用丙酮、石油醚(体积比为6∶4)混合溶剂浸泡中药菊花2h,超声振荡30min,过滤;滤液经C18柱、石墨碳柱固相萃取、净化。采用电子捕获检测器、程序升温、SPB-5(30m×0.25mm×0.25μm)毛细管柱气相色谱检测技术对菊花中12种农药残留进行分析。结果表明,12种农药残留在22min内均可很好地得以分离,最低检出浓度为0.01~0.05mg/L;12种农药的添加回收率为74.7%~100.6%,线性范围为0.1~10.0mg/L,线性相关系数r2≥0.9922。本文建立了中药菊花中12种农药残留量的气相色谱分析方法,符合农药多残留分析的要求。
【Abstract】 In this paper, the author has established an analysis method in quantitative determination of the 12 kinds of organophosphate and organochlorine pesticides, including op′-DDD, pp′-DDD, op′-DDT, pp′-DDT, α-BHC, β-BHC, γ-BHC, δ-BHC, quintozene, fenthion, malathion and parathion-methyl residues in the Dendranthema moriflolium. The sample for analysis has been dipped from the acetone-petroleum ether (V∶V=6∶4) for 2 h and ultrasonic shake for 30 min, then it was filtered out. After the extract was purified on a C18 cartridge and graphitic columns, it was collected and evaporated to get dry. The residues were then determined by capillary gas chromatography with ECD and a SPB-5 column (30 m×0.25 mm×0.25 μm). All the above said 12 pesticides were then well separated in 22 min. With the average recoveries of the pesticides being 74.7%-100.6%, the minimum detectable concentration would range from 0.01-0.05 mg/kg and their calibration curves would then be determined within the range of 0.01-10 mg/L. Then it would be found that the correlation coefficient (r2) would not be less than 0.992 2. Thus, it can be concluded that what we have worked out is by nature a multiresidue monitoring method for determining 12 pesticides in Dendranthema moriflolium by capillary gas chromatography, which can meet the requirements of the pesticide multiresidues analysis.
【Key words】 pesticide; Dendranthema moriflolium; solid-phase extraction; pesticide multiresidues; GC;
- 【文献出处】 安全与环境学报 ,Journal of Safety and Environment , 编辑部邮箱 ,2007年02期
- 【分类号】S481.8
- 【被引频次】19
- 【下载频次】644