首页|呋虫胺和唑虫酰胺在茶叶加工过程中的残留特征及膳食风险评估

呋虫胺和唑虫酰胺在茶叶加工过程中的残留特征及膳食风险评估

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为明确呋虫胺和唑虫酰胺微乳剂在茶叶种植、烘干、浸泡过程中的残留特征,在山东、浙江等10地开展规范农药登记残留田间试验,并进行加工因子校正膳食风险评估模型比较研究。样品经体积分数5%甲酸-乙腈提取、盐析分层、分散固相萃取净化后,经超高效液相色谱-串联质谱法检测,外标法定量。结果表明:在0。005~0。500 μg/mL范围内,呋虫胺及其代谢物、唑虫酰胺质量浓度与其响应峰面积呈良好线性关系(R2>0。99),在0。05、1。00、20。00、50。00 mg/kg(茶鲜叶、茶干叶),0。05、0。10、5。00 mg/kg(茶汤)添加水平下,呋虫胺及其代谢物1-甲基-3-[(3-四氢呋喃)甲基]脲、1-甲基-3-[(3-四氢呋喃)甲基]二氢胍盐的平均加标回收率为74%~103%,相对标准偏差为1%~9%;唑虫酰胺的平均加标回收率为75%~95%,相对标准偏差为1%~6%,方法定量限均为0。05 mg/kg;20%呋虫胺·唑虫酰胺微乳剂按推荐剂量施药后,呋虫胺(含代谢物)在茶鲜叶中的规范残留试验中值(supervised trials median residue,STMR)经烘干因子校正后与茶干叶中STMR相应的国家估算每日摄入量(national estimated daily intake,NEDI)均为4。08 mg,占每日允许摄入量(allowable daily intake,ADI)的32。4%;唑虫酰胺在茶鲜叶中的STMR经烘干因子校正后的NEDI为0。175 81 mg,占ADI的46。5%,茶干叶中STMR对应的NEDI为0。189 25 mg,占ADI的50。1%,呋虫胺和唑虫酰胺在不同评估模型下获得的长期膳食暴露风险均低于100%;呋虫胺(含代谢物)经加工因子校正后的国际短期膳食摄入量(international estimation of short-term dietary intake,IESTI)与校正前处于同一风险水平,低于急性参考剂量(acute reference dose,ARfD)(1 mg/kg);唑虫酰胺的IESTI为3。46× 10-4 mg/kg(采收间隔7 d),低于ARfD(0。01 mg/kg),本研究方法在茶汤中未检测到唑虫酰胺残留,故未得到浸泡因子及相应的IESTI。综上,按推荐剂量在茶树上使用20%呋虫胺·唑虫酰胺微乳剂是安全的,最终残留量对应的长期及急性膳食摄入风险均在可接受范围,利用加工因子校正评估模型更切合实际风险水平。
Residual Characteristics and Dietary Risk Assessment of Dinotefuran and Tolfenpyrad in Tea Processing
To clarify the residual characteristics of dinotefuran tolfenpyrad microemulsion during tea planting,drying and brewing,standardized field trials of pesticide registration residues were conducted in 10 provinces including Shandong and Zhejiang.Dietary risk assessment models were compared with and without adjustment of processing factors.The samples were extracted using acetonitrile containing 5%formic acid,salted out,purified by dispersed solid phase extraction,detected by ultra-high performance liquid chromatography-tandem mass spectrometry,and quantified by an external standard method.In the range of 0.005-0.500 μg/mL,a good linear relationship was obtained between the concentrations of dinotefuran and its metabolites as well as tolfenpyrad and their response peak areas(R2>0.99).The average recovery rates of dinotefuran and its metabolites 1-methyl-3-(tetrahydro-3-furylmethyl)guanidine(DN)and 1-methyl-3-(tetrahydro-3-furylmethyl)urea(UF)in fresh and dried tea leaves spiked at 0.05,1.00,20.00 and 50.00 mg/kg and in tea infusion spiked at 0.05,0.10 and 5.00 mg/kg ranged from 74%to 103%,with relative standard deviations(RSDs)of 1%-9%.The spiked recovery rates of tolfenpyrad were between 75%and 95%,with RSDs of 1%-6%.The limit of quantitation(LOQ)was 0.05 mg/kg for all the analytes.In the case of the application of 20%dinotefuran·tolfenpyrad microemulsion at the recommended dose,both the national estimated daily intake(NEDI)for supervised trials median residue(STMR)adjusted with the drying factor of dinotefuran(containing its metabolites)in fresh tea leaves and that in dried tea leaves were 4.08 mg,accounting for 32.4%of the acceptable daily intake(ADI).The NEDI for STMR of tolfenpyrad adjusted with the drying factor in fresh tea leaves was 0.175 81 mg,accounting for 46.5%of the ADI,and the NEDI for STMR of tolfenpyrad in dried tea leaves was 0.189 25 mg,accounting for 50.1%of the ADI.According to different risk assessment models,the long-term exposure risk to both dinotefuran and tolfenpyrad was less than 100%.The national estimated short-term intake(IESTI)of dinotefuran(containing its metabolites)remained at the same risk level before and after processing factor adjustment,which was lower than the acute reference dose(ARfD)of 1 mg/kg.The IESTI of tolfenpyrad was 3.46 x 10-4 mg/kg,which was lower than the ARfD of 0.01 mg/kg,and tolfenpyrad residue was below the detectable level under the method established in this study,so no brewing facter and corresponding IESTI were obtained.In conclusion,the application of 20%dinotefuran·tolfenpyrad microemulsion on tea plants is safe at the recommended dose,and the risk of long-term and acute dietary exposure to dinotefuran and tolfenpyrad residues in tea is within the acceptable range.The risk assessment models with processing factor adjustment are closer to the actual risk level.

dinotefurantolfenpyradtea processing factorsresidual characteristicsrisk assessment

李春勇、吕莹、金静、王霞、秦曙

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山西农业大学山西功能农产品检验检测中心,山西 太原 030031

呋虫胺 唑虫酰胺 茶叶加工因子 残留特征 风险评估

2025

食品科学
北京食品科学研究院

食品科学

北大核心
影响因子:1.327
ISSN:1002-6630
年,卷(期):2025.46(1)