分散固相萃取结合HPLC-MS/MS同时测定茶叶中丁醚脲及其降解产物
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(1. 长沙理工大学化学与生物工程学院,湖南 长沙 410076;2. 湖南出入境检验检疫局,湖南 长沙 410004)

作者简介:

肖利民,男,长沙理工大学讲师,学士。

通讯作者:

戴华(1964—),男,湖南出入境检验检疫局研究员。E-mail:Ddaihua@yeah.net

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Simultaneous determination of diafenthiuron and its degradation products in teas by dispersive solid-phase extraction and high performance liquid chromatography-tandem mass
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(1. School of Chemistry and Biological Engineering, Changsha University of Science and Technology, Changsha, Hunan410076, China; 2. Hunan Entry-Exit Inspection and Quarantine Bureau of China, Changsha, Hunan 410004, China)

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    摘要:

    建立分散固相萃取(QuEChERS)—高效液相色谱—串联质谱(HPLC-MS/MS)法同时测定茶叶中丁醚脲及其降解产物残留量的方法。样品中丁醚脲及其降解产物用乙腈提取,提取液经过分散固相萃取法(QuEChERS) 净化后,采用C18色谱柱分离,以0.1%乙酸水溶液和乙腈为流动相,梯度洗脱,在电喷雾离子源正离子模式下采用质谱多反应监测(MRM)模式检测,外标法定量。结果表明,丁醚脲的定量限为0.01 mg/kg,丁醚脲—甲酰胺的定量限为0.005 mg/kg、丁醚脲—脲的定量限为0.003 mg/kg。在3个浓度水平下平均回收率为62.2%~99.6%;相对标准偏差(RSD%)为1.3%~9.4%。该方法能同时对茶叶中丁醚脲及其降解产物进行定性、定量检测,方法简单、快速,准确度、灵敏度高,且减少了前处理过程中丁醚脲的分解。可同时对茶叶中丁醚脲及其降解产物进行定性、定量检测,满足残留检测的需要。

    Abstract:

    A simple and efficient method based on QuEChERS and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of diafenthiuron and itss degradation products in tea. The sample was extracted with acetonitrile and cleaned up with QuEChERS. In the chromatographic analysis, three target compounds were separated on a C18 column (150 mm × 4.6 mm, 3.5 μm) with the gradient elution using the mobile phases of acetonitrile and water containing 0.1% acetic acid. The mass analyzer was performed using positive scan mode with MRM monitor using external standard method. The results showed that the limits of quantitatiom ( LOQ, S /N≥10) of diafenthiuron, diafenthiuron-methanimidamide and diafenthiuron-urea were 0.01 mg/kg, 0.005 mg/kg, 0.003 mg/kg, respectively. The average recoveries of the three compounds spiked at three level concentration were in the range of 62.2%~99.6%, with the relative standard deviations( RSDs) of 1.3%~9.4%. This method is simple, fast, credible and high sensitivity can be applied to simultaneous identification and quantitation of diafenthiuron and its degradation products in teas, and the same time this method can effectively reducing the degaragation of diafenthiuron in the pretreatment process. This method meet the requirements for determination of diafenthiuron and its degradation products in tea.

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肖利民,王美玲,戴洁芸,等.分散固相萃取结合HPLC-MS/MS同时测定茶叶中丁醚脲及其降解产物[J].食品与机械,2018,34(5):82-86.
XIAOLimin, WANGMeiling, DAIJieyun, et al. Simultaneous determination of diafenthiuron and its degradation products in teas by dispersive solid-phase extraction and high performance liquid chromatography-tandem mass[J]. Food & Machinery,2018,34(5):82-86.

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  • 收稿日期:2018-02-03
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  • 在线发布日期: 2023-03-17
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