氟啶虫酰胺在茶叶中的残留分析及膳食摄入风险评估

Residue analysis and dietary intake risk assessment of flonicamid in tea

中文关键词:  茶叶  氟啶虫酰胺  残留  膳食风险

英文关键词:tea  flonicamid  residue  dietary intake risk assessment

中文摘要:

      目的 建立茶叶中氟啶虫酰胺残留的分析方法, 并评估其在茶叶中的膳食摄入风险。方法 采用乙腈提取茶叶中的氟啶虫酰胺残留, 通过无水MgSO4和乙酸钠进行盐析除水。上清液经无水MgSO4、C18、乙二胺-N-丙基硅烷(primary-secondary amine, PSA)、石墨化炭黑(graphitized carbon black, GCB)吸附净化剂净化, 使用超高效液相色谱-串联质谱法进行分析。检测采用多反应离子监测模式检测, 正离子化, 基质匹配外标法定量。基于残留试验结果和我国人群的膳食结构, 进行膳食摄入风险评估。结果 氟啶虫酰胺在一定质量浓度范围内具有良好的线性关系(r≥0.9999)。在0.01、0.50、20.00和30.00 mg/kg添加水平下, 干茶叶和鲜茶叶中的平均回收率为83.9%~93.6%, 相对标准偏差为1.1%~5.3%。定量限为0.01 mg/kg。最终残留试验和消解试验表明, 氟啶虫酰胺在茶叶上的残留量主要受施药剂量和采收间隔期的共同影响。氟啶虫酰胺在各地鲜茶叶和干茶叶的半衰期分别为0.8~4.0 d和0.8~5.1 d之间, 属于易降解农药。膳食评估的结果为: 通过茶叶摄入氟啶虫酰胺在18岁以上成年人的估算每日摄入量在0.74~0.81 μg/(kg·bw·d)之间, 占日允许摄入量的1.05%~1.16%; 结合我国农药登记情况和现有残留限量, 一般人群氟啶虫酰胺的国家估算每日摄入量为58.5193 μg/(kg·bw·d), 占日允许摄入量的83.6%。氟啶虫酰胺急性毒性低, 导致急性膳食风险的概率较小, 因此无需进行急性膳食风险评估。结论 该方法前处理操作简单, 准确度和灵敏度高, 可用于茶叶上氟啶虫酰胺的残留检测。经评估, 氟啶虫酰胺对一般人群不会产生不可接受风险。

英文摘要:

      Objective To establish an analytical method for the determination of flonicamid residues in tea and assess the dietary intake risk of flonicamid in tea. Methods Flonicamid residues in tea were extracted using acetonitrile, followed by dehydration and salting out with anhydrous MgSO4 and sodium acetate. The supernatant was purified using anhydrous MgSO4, C18, primary-secondary amine (PSA), and graphitized carbon black (GCB) as adsorbents. Analysis was performed using ultra performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode with positive ionization. Quantification was achieved using matrix-matched external standards. Dietary intake risk assessment was conducted based on residue trial results and the dietary structure of the Chinese population. Results Flonicamid had a good linear relationship (r≥0.9999) within a certain concentration range. At levels of 0.01, 0.50, 20.00 and 30.00 mg/kg, the average recovery rates of tea (dry and fresh) ranged from 83.9%–93.6%, with relative standard deviations of 1.1%–5.3%. The limit of quantitation was 0.01 mg/kg. The final residue test and degradation test showed that the residual amount of flonicamid on tea was mainly affected by the combined effects of application dose and harvesting interval. The half-lives of flonicamid in fresh and dry tea in various regions were between 0.8–4.0 d and 0.8–5.1 d, respectively, indicating that it was an easily degradable pesticide. The results of the dietary assessment showed that the estimated daily intake of flonicamid through tea consumption for adults over 18 years old was between 0.74–0.81 μg/(kg·bw·d), which accounted for 1.05% to 1.16% of acceptable daily intake; combining the registration status of pesticides in China and the existing residue limits, the national estimated daily intake of flonicamid for the general population was 58.5193 μg/(kg·bw·d), which accounted for 83.6% of the acceptable daily intake. Flonicamid had low acute toxicity, and the probability of causing acute dietary risk was minimal. Therefore, there was no need to conduct an acute dietary risk assessment. Conclusion This method has simple pretreatment steps, high accuracy and high sensitivity, and can be used for the detection of flonicamid residues in tea. Upon evaluation, it has been determined that flonicamid does not pose an unacceptable risk to the general population.