Determination of residue of silthiopham in wheat by gas chromatography-mass spectrometry method
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摘要: 硅噻菌胺是一种专一防治小麦全蚀病的新型杀菌剂。利用气相色谱-质谱(GC-MS)联用技术建立了一种高效准确的检测小麦中硅噻菌胺残留的方法。样品经乙腈萃取、Florisil固相萃取柱净化后,利用GC-MS检测。结果表明:预处理后样品中硅噻菌胺GC-MS保留时间为7.188 min,在加标量分别为0.001、0.01、0.025 mg时,其平均回收率分别为103.3%、86.5%、80.9%,相对标准偏差(RSD)为7.50%、5.11%、3.52%。该方法在0.0060.1 mg/kg范围内具有较好的线性关系(R2=0.9998),最低检测限(LOD)为0.002 mg/kg,定量限(LOQ)为0.006 mg/kg。该研究为小麦中硅噻菌胺残留提供了一种简便快速有效的检测方法。Abstract: Silthiopham is a new exclusive fungicide for take-all disease of wheat.An efficient and accurate analytical approach was developed for the residue of silthiopham in wheat by gas chromatography-mass spectrometry ( GC-MS) technique.Samples were extracted with acetonitrile and purified via solid phase extraction column ( Florisil) . Then those purified samples were detected by GC-MS. The results indicated that the retention time ( RT) of silthiopham was 7.188 min. And at the amount of standard sample of 0.001, 0.01 and 0.025 mg, the average recovery rate of silthiopham were 103.3%, 86.5%, 80.9%, respectively, with the relative standard deviation ( RSD) 7.50%, 5.11%, 3.52%, separately.The linear ranges were from 0.006 to0.1 mg/kg with a good linear relationship ( R2= 0.9998) .The limit of detection was 0.002 mg/kg, and the limit of quantification was 0.006 mg/kg.Thus, this study provided a simple, rapid and effective method in determination of the residue of silthiopham in wheat.
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Keywords:
- silthiopham /
- gas chromatography-mass spectrometry (GC-MS) /
- wheat /
- residue
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