摘要
目的建立Qu ECh ERS-气相色谱法同时测定果蔬中12种有机氯及拟除虫菊酯类农药残留的方法。方法样品经1%冰乙酸-乙腈均质提取,N-丙基乙二胺(PSA)、ODSC18粉和石墨化碳黑(GCB)粉混合净化后,采用DB-5毛细管柱进行分离,μECD检测器检测,气相色谱法测定,外标法定量。结果 12种农药的浓度为0.025μg/ml^2.5μg/ml时,线性关系良好,相关系数(r)≥0.992。在0.05 mg/kg、0.25 mg/kg、0.50 mg/kg 3种添加水平下,方法的平均回收率为80.21%~113.20%,相对标准偏差(RSD)为3.21%~12.67%(n=6),检出限(LOD)为0.000 2 mg/kg^0.001 0 mg/kg。结论本方法操作简便、定量准确、快速,可满足果蔬中12种有机氯及拟除虫菊酯类农药残留的检测需求。
Objective To establish a method for detecting 12 kinds of organochlorine pesticides and pyrethroid pesticides residues in fruits and vegetables by Qu ECh ERS-gas chromatography spectrometry. Methods Samples were extracted with acetonitrile containing 1% acetate and cleaned up by PSA,ODSC18 and graphitized carbon black（ GCB）. Finally the samples were separated with DB-5 capillary column,determined by gas chromatography and quantified by external standard method. Results When the linear ranges of the method were among 0. 025 μg / ml-2. 5 μg / ml,good linearity was obtained with the correlation coefficients（ r） ≥0. 992. The average recovery rates were among 80. 21%-113. 20%,and relative standard deviations were among3. 21%-12. 67%（ n = 6） at the spiked levels of 0. 05 mg / kg,0. 25 mg / kg and 0. 50 mg / kg,the limits of detection were among 0. 000 2 mg / kg-0. 001 0 mg / kg. Conclusion The method is convenient,accurate,rapid and it could meet the requirement for the determination of 12 kinds of organochlorine pesticides and pyrethroid pesticides residues in fruits and vegetables.
出处
《中国卫生检验杂志》
CAS
2016年第5期619-621,627,共4页
Chinese Journal of Health Laboratory Technology
基金
新疆维吾尔自治区自然基金资助项目(201442137-23)
