UPLC-MS/MS法检测小麦中苯磺隆的残留量
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摘要
通过对苯磺隆检测方法的研究,开发出一种快速、高效测定小麦中苯磺隆残留量的液相色谱-质谱/质谱(UPLC-MS/MS)方法。该方法采用乙腈溶液超声提取小麦中残留的苯磺隆,提取液经过高速离心,通过C18固相萃取柱净化,经UPLC-MS/MS分析测定。该方法最低检出限为1.0μg/kg,线性范围为0.5～50.0ng/ml,加标回收率为93.93%～98.18%,相对标准偏差为1.10%～2.39%。建立了更为准确、快速、灵敏度更高的检测小麦中苯磺隆含量的方法。
A high performance UPLC-MS/MS method for the determination of tribenuron methyl residues in wheat was studied.The tribenuron methyl was extracted through ultrasonic by acetonitrile solution.The extract was purified by C18 solid phase extraction cartridge after high-speed centrifugation.Then it was analyzed by UPLC-MS/MS.The results showed that the minimum detection limit was 1.0μg/kg,the linear range was 0.5-50.0 ng/ml,the recovery of standard addition was 93.93%-98.18%,and the relative standard deviation was 1.10%-2.39%.In conclusion,we established a more accurate,rapid and sensitive method for detecting the tribenuron methyl residues in wheat.
A high performance UPLC-MS/MS method for the determination of tribenuron methyl residues in wheat was studied.The tribenuron methyl was extracted through ultrasonic by acetonitrile solution.The extract was purified by C18 solid phase extraction cartridge after high-speed centrifugation.Then it was analyzed by UPLC-MS/MS.The results showed that the minimum detection limit was 1.0μg/kg,the linear range was 0.5-50.0 ng/ml,the recovery of standard addition was 93.93%-98.18%,and the relative standard deviation was 1.10%-2.39%.In conclusion,we established a more accurate,rapid and sensitive method for detecting the tribenuron methyl residues in wheat.
引文
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[4]宋丽娟,许满军.LC-MS/MS法检验土壤中的磺酰脲类和磺酰胺类除草剂[J].刑事技术,2015,40(5):382-387.
[5]吴春英,白鹭,谷风,等.固相萃取-超高效液相色谱/串联质谱法同时测定水中27种磺酰脲类除草剂[J].分析科学学报,2016,32(6):783-788.
[2]李西鹏.苯磺隆对小麦田杂草的抗性监测研究分析[J].河南农业,2014(1):29.
[3]刘海林,耿安静,陆晓宇,等.LC-MS/MS测定蔬菜中残留的磺酰脲类除草剂[J].江苏农业科学,2015,43(7):325-327.
[4]宋丽娟,许满军.LC-MS/MS法检验土壤中的磺酰脲类和磺酰胺类除草剂[J].刑事技术,2015,40(5):382-387.
[5]吴春英,白鹭,谷风,等.固相萃取-超高效液相色谱/串联质谱法同时测定水中27种磺酰脲类除草剂[J].分析科学学报,2016,32(6):783-788.