Acta Agriculturae Zhejiangensis ›› 2026, Vol. 38 ›› Issue (3): 581-587.DOI: 10.3969/j.issn.1004-1524.20250071
• Quality and Safety of Agricultural Products • Previous Articles Next Articles
DING Peiheng1(
), YU Fei1,2, CHENG Ke1,2, WANG Chenxue1, ZHENG Xiao1, MU Wenjing1,*(
), WANG Xiuguo1
Received:2025-01-22
Online:2026-03-25
Published:2026-04-17
Contact:
MU Wenjing
CLC Number:
DING Peiheng, YU Fei, CHENG Ke, WANG Chenxue, ZHENG Xiao, MU Wenjing, WANG Xiuguo. Residual degradation and dietary risk assessment of tolfenpyrad and flonicamid in tea leaves[J]. Acta Agriculturae Zhejiangensis, 2026, 38(3): 581-587.
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URL: http://www.zjnyxb.cn/EN/10.3969/j.issn.1004-1524.20250071
| 农药 Pesticide | 保留时间/min Retention time/min | 定性离子对 Qualitative ion pair(m/z) | 定量离子对 Quantitative ion pair(m/z) | 管透镜电压/V Tube lens voltage/V | 碰撞能量/eV Collision energy/eV |
|---|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 3.2 | 384.2/154.1 | 384.2/197.1 | 200 | 38/22 |
| 氟啶虫酰胺Flonicamid | 2.3 | 230.2/174.1 | 230.2/203.1 | 73 | 17/16 |
Table 1 Ion pair information for qualitative and quantitative analysis of tolfenpyrad and flonicamid
| 农药 Pesticide | 保留时间/min Retention time/min | 定性离子对 Qualitative ion pair(m/z) | 定量离子对 Quantitative ion pair(m/z) | 管透镜电压/V Tube lens voltage/V | 碰撞能量/eV Collision energy/eV |
|---|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 3.2 | 384.2/154.1 | 384.2/197.1 | 200 | 38/22 |
| 氟啶虫酰胺Flonicamid | 2.3 | 230.2/174.1 | 230.2/203.1 | 73 | 17/16 |
| 农药 Pesticide | 工作液 Working solution | 线性方程 Linear equation | 决定系数(R2) Coefficient of determination(R2) |
|---|---|---|---|
| 唑虫酰胺 Tolfenpyrad | 乙腈Acetonitrile | y=1 776 319x+4 070 | 0.999 7 |
| 茶叶(鲜)空白基质Fresh tea blank substrate | y=1 056 435x+3 187 | 0.998 7 | |
| 茶叶(干)空白基质Dry tea blank substrate | y=930 132x+6 845 | 0.998 8 | |
| 氟啶虫酰胺 Flonicamid | 乙腈Acetonitrile | y=1 901 204x+5 224 | 0.999 6 |
| 茶叶(鲜)空白基质Fresh tea blank substrate | y=1 255 664x+4 587 | 0.999 9 | |
| 茶叶(干)空白基质Dry tea blank substrate | y=1 124 471x+5 783 | 0.999 9 |
Table 2 Validation of detection methods for tolfenpyrad and flonicamid
| 农药 Pesticide | 工作液 Working solution | 线性方程 Linear equation | 决定系数(R2) Coefficient of determination(R2) |
|---|---|---|---|
| 唑虫酰胺 Tolfenpyrad | 乙腈Acetonitrile | y=1 776 319x+4 070 | 0.999 7 |
| 茶叶(鲜)空白基质Fresh tea blank substrate | y=1 056 435x+3 187 | 0.998 7 | |
| 茶叶(干)空白基质Dry tea blank substrate | y=930 132x+6 845 | 0.998 8 | |
| 氟啶虫酰胺 Flonicamid | 乙腈Acetonitrile | y=1 901 204x+5 224 | 0.999 6 |
| 茶叶(鲜)空白基质Fresh tea blank substrate | y=1 255 664x+4 587 | 0.999 9 | |
| 茶叶(干)空白基质Dry tea blank substrate | y=1 124 471x+5 783 | 0.999 9 |
| 农药 Pesticide | 基质 Substrate | 添加浓度 Added concentration/(mg·kg-1) | 平均回收率/% Average recovery rate/% | RSD/% |
|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 茶叶(鲜)Fresh tea | 0.05 | 81 | 4.2 |
| 5.00 | 85 | 3.2 | ||
| 50.00 | 88 | 2.2 | ||
| 茶叶(干)Dry tea | 0.05 | 86 | 5.3 | |
| 5.00 | 85 | 4.7 | ||
| 50.00 | 92 | 2.1 | ||
| 氟啶虫酰胺Flonicamid | 茶叶(鲜)Fresh tea | 0.05 | 88 | 6.0 |
| 5.00 | 89 | 3.9 | ||
| 20.00 | 96 | 4.4 | ||
| 茶叶(干)Dry tea | 0.05 | 90 | 2.3 | |
| 5.00 | 90 | 2.9 | ||
| 20.00 | 93 | 2.3 |
Table 3 Recovery rates and relative standard deviation (RSD)of tolfenpyrad and flonicamid in tea samples
| 农药 Pesticide | 基质 Substrate | 添加浓度 Added concentration/(mg·kg-1) | 平均回收率/% Average recovery rate/% | RSD/% |
|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 茶叶(鲜)Fresh tea | 0.05 | 81 | 4.2 |
| 5.00 | 85 | 3.2 | ||
| 50.00 | 88 | 2.2 | ||
| 茶叶(干)Dry tea | 0.05 | 86 | 5.3 | |
| 5.00 | 85 | 4.7 | ||
| 50.00 | 92 | 2.1 | ||
| 氟啶虫酰胺Flonicamid | 茶叶(鲜)Fresh tea | 0.05 | 88 | 6.0 |
| 5.00 | 89 | 3.9 | ||
| 20.00 | 96 | 4.4 | ||
| 茶叶(干)Dry tea | 0.05 | 90 | 2.3 | |
| 5.00 | 90 | 2.9 | ||
| 20.00 | 93 | 2.3 |
| 农药 Pesticide | 采收间隔期/d Harvest interval/d | 基质 Substrate | 残留中值/(mg·kg-1) Supervised trials median residue/(mg·kg-1) | 最高残留量/(mg·kg-1) Highest residue/(mg·kg-1) |
|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 7 | 茶叶(鲜)Fresh tea | 1.10 | 5.00 |
| 茶叶(干)Dry tea | 1.60 | 5.20 | ||
| 10 | 茶叶(鲜)Fresh tea | 0.62 | 2.50 | |
| 茶叶(干)Dry tea | 0.83 | 4.60 | ||
| 氟啶虫酰胺Flonicamid | 7 | 茶叶(鲜)Fresh tea | 0.19 | 0.58 |
| 茶叶(干)Dry tea | 0.24 | 0.90 | ||
| 10 | 茶叶(鲜)Fresh tea | 0.18 | 0.37 | |
| 茶叶(干)Dry tea | 0.14 | 0.55 |
Table 4 Final residue test results of tolfenpyrad and flonicamid
| 农药 Pesticide | 采收间隔期/d Harvest interval/d | 基质 Substrate | 残留中值/(mg·kg-1) Supervised trials median residue/(mg·kg-1) | 最高残留量/(mg·kg-1) Highest residue/(mg·kg-1) |
|---|---|---|---|---|
| 唑虫酰胺Tolfenpyrad | 7 | 茶叶(鲜)Fresh tea | 1.10 | 5.00 |
| 茶叶(干)Dry tea | 1.60 | 5.20 | ||
| 10 | 茶叶(鲜)Fresh tea | 0.62 | 2.50 | |
| 茶叶(干)Dry tea | 0.83 | 4.60 | ||
| 氟啶虫酰胺Flonicamid | 7 | 茶叶(鲜)Fresh tea | 0.19 | 0.58 |
| 茶叶(干)Dry tea | 0.24 | 0.90 | ||
| 10 | 茶叶(鲜)Fresh tea | 0.18 | 0.37 | |
| 茶叶(干)Dry tea | 0.14 | 0.55 |
| 食物种类 Food classification | 登记作物 Registration crop | 膳食量/kg Dietary intake/kg | 参考限量/(mg·kg-1) Reference limit/(mg·kg-1) | 限量来源 Limited source | NEDI/mg |
|---|---|---|---|---|---|
| 浅色蔬菜Light vegetables | 甘蓝Cabbage | 0.183 7 | 0.5 | 中国China | 0.091 85 |
| 水果Fruits | 柑橘Citrus | 0.045 7 | 0.8 | 美国America | 0.036 56 |
| 饮料类Beverages | 茶Tea | 0.012 0 | 1.6 | STMR | 0.019 20 |
| 合计Total | — | 0.241 4 | — | — | 0.147 61 |
Table 5 The chronic dietary risk assessment of tolfenpyrad at recommended dose
| 食物种类 Food classification | 登记作物 Registration crop | 膳食量/kg Dietary intake/kg | 参考限量/(mg·kg-1) Reference limit/(mg·kg-1) | 限量来源 Limited source | NEDI/mg |
|---|---|---|---|---|---|
| 浅色蔬菜Light vegetables | 甘蓝Cabbage | 0.183 7 | 0.5 | 中国China | 0.091 85 |
| 水果Fruits | 柑橘Citrus | 0.045 7 | 0.8 | 美国America | 0.036 56 |
| 饮料类Beverages | 茶Tea | 0.012 0 | 1.6 | STMR | 0.019 20 |
| 合计Total | — | 0.241 4 | — | — | 0.147 61 |
| 食物种类 Food classification | 登记作物 Registration crop | 膳食量 Dietary intake/kg | 参考限量 Reference limit/(mg·kg-1) | 限量来源 Limited source | NEDI/mg |
|---|---|---|---|---|---|
| 米及其制品Rice and its products | 稻谷Rice | 0.239 9 | 0.50 | 中国China | 0.119 95 |
| 薯类Tubers | 马铃薯Potato | 0.049 5 | 0.20 | 中国China | 0.009 90 |
| 深色蔬菜Dark vegetables | 菠菜Spinach | 0.091 5 | 20.00 | 中国China | 1.830 00 |
| 浅色蔬菜Light vegetables | 甘蓝Cabbage | 0.183 7 | 2.00 | 中国China | 0.367 40 |
| 水果Fruits | 苹果Apple | 0.045 7 | 1.00 | 中国China | 0.045 70 |
| 植物油Vegetable oil | 棉籽Cottonseed | 0.032 7 | 0.60 | 中国China | 0.019 62 |
| 食盐Salt | 茶Tea | 0.012 0 | 0.24 | STMR | 0.002 88 |
| 酱油Soy sauce | 大葱Shallot | 0.009 0 | 0.03 | 欧盟EU | 0.000 27 |
| 合计Total | — | 0.664 0 | — | — | 2.395 72 |
Table 6 The chronic dietary risk assessment of flonicamid at recommended dose
| 食物种类 Food classification | 登记作物 Registration crop | 膳食量 Dietary intake/kg | 参考限量 Reference limit/(mg·kg-1) | 限量来源 Limited source | NEDI/mg |
|---|---|---|---|---|---|
| 米及其制品Rice and its products | 稻谷Rice | 0.239 9 | 0.50 | 中国China | 0.119 95 |
| 薯类Tubers | 马铃薯Potato | 0.049 5 | 0.20 | 中国China | 0.009 90 |
| 深色蔬菜Dark vegetables | 菠菜Spinach | 0.091 5 | 20.00 | 中国China | 1.830 00 |
| 浅色蔬菜Light vegetables | 甘蓝Cabbage | 0.183 7 | 2.00 | 中国China | 0.367 40 |
| 水果Fruits | 苹果Apple | 0.045 7 | 1.00 | 中国China | 0.045 70 |
| 植物油Vegetable oil | 棉籽Cottonseed | 0.032 7 | 0.60 | 中国China | 0.019 62 |
| 食盐Salt | 茶Tea | 0.012 0 | 0.24 | STMR | 0.002 88 |
| 酱油Soy sauce | 大葱Shallot | 0.009 0 | 0.03 | 欧盟EU | 0.000 27 |
| 合计Total | — | 0.664 0 | — | — | 2.395 72 |
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