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超声提取-气相色谱法测定高粱中腈菌唑与烯唑醇农药残留量

2019-07-08陈顺琴杨晖王爱民

湖北农业科学 2019年10期

陈顺琴 杨晖 王爱民

摘要:利用超声提取-气相色谱法测定高粱中腈菌唑与烯唑醇农药残留。高粱样品用不同比例的乙腈-丙酮进行提取,弗洛里硅藻土净化,旋转蒸发浓缩,最后采用气相色谱-电子捕获检测器(ECD)进行测定。腈菌唑农药线性范围为0.012 5~0.400 μg/g,方法检出限(3S/N)为0.002 μg/g,相对标准偏差(n=6)RSD为3.7%;烯唑醇农药线性范围为0.004 76~0.152 μg/g,方法检出限(3S/N)为0.000 83 μg/g,相对标准偏差(n=6)RSD为1.2%。该方法简单、高效、快速、灵敏,能满足高粱中腈菌唑与烯唑醇农药残留量的测定。

关键词:气相色谱法;超声提取;腈菌唑;烯唑醇;高粱

中图分类号:S132         文献标识码:A

文章编号:0439-8114(2019)10-0146-04

Abstract: A method of ultrasonic assisted extraction combined with gas chromatography was used to determine pesticide residue of myclobutanil and diniconazole in sorghum.The sample was extracted by a mixture of acetonitrile and acetone,then purified with concentrated flory diatomite acid,concentrated with rotary evaporation,and analyzed with GC-ECD. Linearity range of myclobutanil was found between 0.012 5~0.400 μg/g,and the detection limit(3S/N) was 0.002 μg/g,and the values of RSD(n=6) was 3.7%;Linearity range of diniconazole was found between 0.004 76~0.152 μg/g,and the detection limit(3S/N) was 0.000 83 μg/g,and the values of RSD(n=6) was 1.2%. This developed method is simple,quickness,rapid,sensitive and can therefore be used for the determination of myclobutanil and diniconazole in sorghum.

Key words: gas chromatograph;ultrasonic assisted extraction;myclobutanil;diniconazole;sorghum

腈菌唑、烯唑醇均屬于高效、低毒、广谱的新型三唑类杀菌剂农药,主要对病原菌的麦角甾醇的生物合成起抑制作用,对子囊菌、担子菌均具有较好的防治作用[1,2]。腈菌唑化学名称为2-(4-氯苯基)-2-(IH-1,2,4三唑甲基)己腈[3];烯唑醇又名病除净、速保利、特谱唑,化学名字为(E)-1-(2,4-二氯苯基)-4,4-二甲基-2-(1,2,4-三唑-1-基)-1-戊烯-3-醇[3]。该类杀菌剂主要用于防治谷物叶部和穗部病害,如霜霉病、斑枯病、萎凋病、黑粉病、腹黑病、锈病、疮痂病等;在种子处理中用于预防治黑粉菌、腥黑粉菌和腔菌导致的病害;也可防治葡萄的霜霉病,玫瑰的霜霉病、锈病和黑斑病,花生的叶斑病,香蕉叶斑病和咖啡锈病;也用于果树、蔬菜和其他观赏植物。这类杀菌剂具有极高的杀菌活性、内吸性强、持效期长,兼有预防与治疗的作用,是一种高活性的植物生长调节剂和杀菌剂。但其对人体的危害不容忽视,很多国家已经明确限定该农药在食品中的最高残留量[4]。……

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