超高效液相色谱-三重四极杆串联质谱法分析茶叶中联苯肼酯残留与风险评估

Risk Assessment and Residue Analysis of Bifenazate in Tea by UPLC-MS/MS

  • 摘要: 建立了QuEChERS分散固相萃取技术净化茶叶,超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)法测定茶叶鲜叶和成茶中联苯肼酯残留的分析方法。利用该方法研究了43%联苯肼酯悬浮剂在茶叶鲜叶生长中的残留降解规律,并对其在茶叶饮用中的安全性进行了风险评估。结果表明,联苯肼酯在0.002 5~1.00 mg/L浓度范围内的线性关系良好,相关系数r为0.994 2。在0.020、0.20、2.0 mg/kg添加浓度下,绿茶中联苯肼酯的平均回收率分别为79.3%、88.6%、103.4%,相对标准偏差(RSD)分别为6.1%、5.9%、3.7%;红茶中联苯肼酯的平均回收率分别为79.3%、82.6%、103.3%,RSD分别为6.7%、4.5%、4.7%;鲜叶中联苯肼酯的平均回收率分别为91.1%、94.4%、91.0%,RSD分别为4.3%、3.8%、7.6%。方法检出限(LOD,S/N=3)为1.5 μg/kg,定量限(LOQ,S/N=10)为5 μg/kg。由于不同地区和时间的茶叶生长稀释作用、气候温度的不同,43%联苯肼酯悬浮剂在茶鲜叶生长中半衰期为1.4~2.9天;按照推荐剂量和1.5倍推荐剂量施药1~2次,结果表明,10天后成茶中的联苯肼酯残留量均小于5 mg/kg。根据风险评估结果,建议我国茶叶中联苯肼酯最大残留限量(MRL)值可设为5 mg/kg。

     

    Abstract: A convenient and sensitive residue analysis method for bifenazate in fresh tea leaves and made tea was developed and validated by ultra high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UPLC-MS/MS) followed by dispersive solid phase extraction cleanup. The calibration curve is linear over the concentration of 0.002 5-1.00 mg/L for bifenazate with the correlation coefficient (r) of 0.994 2. The average recoveries of bifenazate at three spiked concentration levels (0.020, 0.20, 2.0 mg/kg) in green tea sample matrixes are 79.3%, 88.6% and 103.4% with the relative standard deviations (RSDs) of 6.1%, 5.9% and 3.7%, in black tea sample matrixes are 79.3%, 82.6% and 103.3% with RSDs of 6.7%, 4.5% and 4.7%, in fresh tea leaves are 91.1%, 94.4% and 91.0% with RSDs of 4.3%, 3.8% and 7.6%, respectively. The limit of detection (LOD, S/N=3) of befenazate is 1.5 μg/kg,and the limit of quantitation (LOQ, S/N=10) of bifenazate in different matrixes is 5 μg/kg. This proposed method was successfully applied in the degradation and final residue study of 43% bifenazate suspension concentrate (SC) in the field treatment experiment. The degradation half-life time of bifenazate in fresh tea leaves is in the range of 1.4-2.9 days. According to the recommended dose and the 1.5 times of recommended dose after 1-2 times, the results show that the final residual amount of bifenazate in made tea after 10 days is less than 5 mg/kg. According to the results of risk assessment, it is suggested that the maximum residue limit (MRL) of bifenazate in tea can be set to 5 mg/kg for tea drinking with the pre-harvest intervals (PHI) of 10 days, this is a safety threshold for the human body.

     

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