固相萃取-气相色谱法同时检测草莓中13种 农药残留
目的 建立一种固相萃取-毛细管柱气相色谱方法, 可以同时检测草莓中常用的13种农药残留, 包括百菌清、腐霉利、粉唑醇、腈菌唑、醚菌酯、苯醚甲环唑、烯酰吗啉等7种杀菌剂, 毒死蜱、三氟氯氰菊酯、哒螨灵、氰戊菊酯等4种杀虫剂及莠去津、乙草胺等2种除草剂。方法 草莓样品20 g匀浆后, 经乙腈50 mL提取, NH2固相萃取柱净化, HP-5毛细管气相色谱柱进行分离, GC-ECD 进行定性及定量分析。结果 13 种农药残留的色谱图分离效果良好, 线性相关系数均大于0.996, 方法检出限在0.01 mg/kg~0.5 mg/kg之间。13种农药的添加水平为0.01 mg/kg~2 mg/kg, 回收试验表明该方法平均回收率在70.5%~114.5%之间, 相对标准偏差在2.17%~6.85%之间。结论 该方法简单、快速、灵敏、净化效果好、回收率高, 适合草莓中多种农药残留的检测和安全监控。通过对50份草莓样品进行检测, 检出百菌清、乙草胺、毒死蜱、粉唑醇、醚菌酯、烯酰吗啉6种农药。
Objective To established a solid phase extraction-capillary gas chromatography method for the determination of 13 pesticides multi-residues in strawberry, including seven fungicides such as chlorothalonil, procymidone, flutriafol, myclobutanil, kresoxim-methyl, difenoconazole and dimethomorph; four insecti-cides such as chlorpyrifos, cyhalothrin, pyridaben and fenvalerate; two herbicides such as atrazine and ace-tochlor. Methods After the homogenized strawberry samples with 20 g were extracted with acetonitrile by 50 mL and purified with NH2 solid-phase extraction column, the samples were separated by HP-5 gas chromatography column and detected with GC-ECD. Results A good separation for 13 pesticides was achieved using the established method, with correlation coefficients above 0.996. The detection limit of the method was 0.01~0.5 mg/kg. Shown as the addition recovery experiments, the method average recoveries of the 13 pesticides ranged from 70.5% to 114.5% in the range of 0.01 mg/kg~2 mg/kg. The relative standard deviation was 2.17%~6.85%. Conclusion The method showed simple, rapid, and sensitive, with good purifying effect and high recovery rate, and was suitable for the detection and security monitoring of pesticide residues in strawberry. Six kinds of pesticides, chlorothalonil, chlorpyrifos, acetochlor, flutriafol, kresoxim methyl, and dimethomorph, were found through the detection in 50 strawberry samples.
标题：固相萃取-气相色谱法同时检测草莓中13种 农药残留
英文标题：Simultaneous determination for the residue of thirteen pesticides in strawberry with solid phase extraction and gas chromatography
作者：
袁烁 北京农学院
赵建庄 北京农学院
蔡慧敏 北京农学院
贾临芳 北京农学院
梁丹 北京农学院
魏朝俊 北京农学院
中文关键词:草莓,固相萃取,气相色谱法,农药残留,
英文关键词:strawberry,solid-phase extraction,gas chromatography,pesticide residues,
发表日期：2014-08-21
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