Acta Agriculturae Zhejiangensis ›› 2021, Vol. 33 ›› Issue (7): 1292-1299.DOI: 10.3969/j.issn.1004-1524.2021.07.15
• Quality and Safety of Agricultural Products • Previous Articles Next Articles
SUN Caixia1(
), OUYANG Zhizhou2,3, LIU Yuhong1, YU Guoguang1
Received:2020-07-26
Online:2021-07-25
Published:2021-08-06
CLC Number:
SUN Caixia, OUYANG Zhizhou, LIU Yuhong, YU Guoguang. Residue dynamic and risk assessment of three fungicides in broccoli[J]. Acta Agriculturae Zhejiangensis, 2021, 33(7): 1292-1299.
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URL: http://www.zjnyxb.cn/EN/10.3969/j.issn.1004-1524.2021.07.15
| 农药 Pesticide | 施用量Application amount | 有效成分用量Active ingredient dosage | ||
|---|---|---|---|---|
| 1.0倍用药 1.0 time the pesticide | 1.5倍用药 1.5 times the pesticide | 1.0倍用药 1.0 time the pesticide | 1.5倍用药 1.5 times the pesticide | |
| 苯醚甲环唑(10%水分散剂) | 40.00 | 60.00 | 4.00 | 6.00 |
| Difenoconazole (10% water dispersant) | ||||
| 戊唑醇(30%乳油) Tebuconazole (30% EC) | 15.00 | 22.50 | 4.50 | 6.75 |
| 腈菌唑(25%乳油) Myclobutanil (25% EC) | 40.00 | 60.00 | 10.00 | 15.00 |
Table 1 Application dose of three pesticides g·667 m-2
| 农药 Pesticide | 施用量Application amount | 有效成分用量Active ingredient dosage | ||
|---|---|---|---|---|
| 1.0倍用药 1.0 time the pesticide | 1.5倍用药 1.5 times the pesticide | 1.0倍用药 1.0 time the pesticide | 1.5倍用药 1.5 times the pesticide | |
| 苯醚甲环唑(10%水分散剂) | 40.00 | 60.00 | 4.00 | 6.00 |
| Difenoconazole (10% water dispersant) | ||||
| 戊唑醇(30%乳油) Tebuconazole (30% EC) | 15.00 | 22.50 | 4.50 | 6.75 |
| 腈菌唑(25%乳油) Myclobutanil (25% EC) | 40.00 | 60.00 | 10.00 | 15.00 |
| 农药 Pesticide | 线性范围 Linear range/ (μg·L-1) | 线性方程 Linear equation | 相关系数 Correlation coefficient | 检出限 Detection limit/ (μg·L-1) | 定量限 Limit of quantitation/ (μg·L-1) | RSD/% (n=7) |
|---|---|---|---|---|---|---|
| 苯醚甲环唑Difenoconazole | 5~100 | y=427.52x-29.9 | 0.994 0 | 1.04 | 3.46 | 13.2 |
| 戊唑醇Tebuconazole | 1~100 | y=309.12x+27.5 | 0.995 4 | 0.24 | 0.79 | 11.4 |
| 腈菌唑Myclobutanil | 1~100 | y=643.24x-45.1 | 0.997 6 | 0.14 | 0.46 | 10.3 |
Table 2 Quantitative features of the proposed method for three pesticides
| 农药 Pesticide | 线性范围 Linear range/ (μg·L-1) | 线性方程 Linear equation | 相关系数 Correlation coefficient | 检出限 Detection limit/ (μg·L-1) | 定量限 Limit of quantitation/ (μg·L-1) | RSD/% (n=7) |
|---|---|---|---|---|---|---|
| 苯醚甲环唑Difenoconazole | 5~100 | y=427.52x-29.9 | 0.994 0 | 1.04 | 3.46 | 13.2 |
| 戊唑醇Tebuconazole | 1~100 | y=309.12x+27.5 | 0.995 4 | 0.24 | 0.79 | 11.4 |
| 腈菌唑Myclobutanil | 1~100 | y=643.24x-45.1 | 0.997 6 | 0.14 | 0.46 | 10.3 |
| 农药 Pesticide | 加标浓度 Spiked concentration/(μg·L-1) | 西兰花样品Broccoli sample(n=3) | |
|---|---|---|---|
| 回收率Recovery rate/% | 相对标准偏差RSD/% | ||
| 苯醚甲环唑Difenoconazole | 20 | 88.4 | 12.9 |
| 50 | 117.8 | 2.8 | |
| 100 | 115.1 | 15.6 | |
| 戊唑醇Tebuconazole | 20 | 82.8 | 8.7 |
| 50 | 109.8 | 14.9 | |
| 100 | 116.4 | 10.3 | |
| 腈菌唑Myclobutanil | 20 | 103.4 | 13.1 |
| 50 | 107.6 | 10.3 | |
| 100 | 111.8 | 16.1 | |
Table 3 Results of tests for precision and recovery of three pesticides
| 农药 Pesticide | 加标浓度 Spiked concentration/(μg·L-1) | 西兰花样品Broccoli sample(n=3) | |
|---|---|---|---|
| 回收率Recovery rate/% | 相对标准偏差RSD/% | ||
| 苯醚甲环唑Difenoconazole | 20 | 88.4 | 12.9 |
| 50 | 117.8 | 2.8 | |
| 100 | 115.1 | 15.6 | |
| 戊唑醇Tebuconazole | 20 | 82.8 | 8.7 |
| 50 | 109.8 | 14.9 | |
| 100 | 116.4 | 10.3 | |
| 腈菌唑Myclobutanil | 20 | 103.4 | 13.1 |
| 50 | 107.6 | 10.3 | |
| 100 | 111.8 | 16.1 | |
| 剂量 Dose | 用药次数 Number of medications | 栽培模式 Cultivation mode | 苯醚甲环唑 Difenoconazole | 戊唑醇 Tebuconazole | 腈菌唑 Myclobutanil | |
|---|---|---|---|---|---|---|
| 1.0倍剂量 1.0 time the dose | 1次用药 1 dose | 露地 Open field | 降解方程 Degradation equation | y=0.855+0.154x | y=0.872+0.172x | y=0.877+0.194x |
| r | 0.968 | 0.914 | 0.964 | |||
| T1/2/d | 4.50 | 4.03 | 3.29 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.810+0.150x | y=0.805+0.166x | y=0.839+0.16x | ||
| r | 0.973 | 0.951 | 0.934 | |||
| T1/2/d | 4.62 | 4.17 | 4.33 | |||
| 2次用药 2 dose | 露地 Open field | 降解方程 Degradation equation | y=0.875+0.127x | y=0.836+0.094x | y=0.738+0.112x | |
| r | 0.962 | 0.984 | 0.906 | |||
| T1/2/d | 5.45 | 7.37 | 6.18 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.766+0.122x | y=0.852+0.067x | y=0.821+0.101x | ||
| r | 0.947 | 0.978 | 0.969 | |||
| T1/2/d | 5.68 | 10.34 | 6.86 | |||
| 1.5倍剂量 1.5 times the dose | 1次用药 1 dose | 露地 Open field | 降解方程 Degradation equation | y=0.522+0.136x | y=0.476+0.226x | y=0.539+0.166x |
| r | 0.934 | 0.925 | 0.942 | |||
| T1/2/d | 5.09 | 3.06 | 4.17 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.529+0.125x | y=0.519+0.196x | y=0.533+0.133x | ||
| r | 0.958 | 0.913 | 0.961 | |||
| T1/2/d | 4.58 | 3.53 | 5.21 | |||
| 2次用药 2 dose | 露地 Open field | 降解方程 Degradation equation | y=0.571+0.11x | y=0.632+0.063x | y=0.558+0.078x | |
| r | 0.901 | 0.924 | 0.949 | |||
| T1/2/d | 6.30 | 11 | 8.88 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.556+0.105x | y=0.566+0.059x | y=0.616+0.069x | ||
| r | 0.922 | 0.947 | 0.933 | |||
| T1/2/d | 6.60 | 11.74 | 10.04 |
Table 4 Residue degradation dynamic of three pesticides in broccoli under greenhouse and open fields
| 剂量 Dose | 用药次数 Number of medications | 栽培模式 Cultivation mode | 苯醚甲环唑 Difenoconazole | 戊唑醇 Tebuconazole | 腈菌唑 Myclobutanil | |
|---|---|---|---|---|---|---|
| 1.0倍剂量 1.0 time the dose | 1次用药 1 dose | 露地 Open field | 降解方程 Degradation equation | y=0.855+0.154x | y=0.872+0.172x | y=0.877+0.194x |
| r | 0.968 | 0.914 | 0.964 | |||
| T1/2/d | 4.50 | 4.03 | 3.29 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.810+0.150x | y=0.805+0.166x | y=0.839+0.16x | ||
| r | 0.973 | 0.951 | 0.934 | |||
| T1/2/d | 4.62 | 4.17 | 4.33 | |||
| 2次用药 2 dose | 露地 Open field | 降解方程 Degradation equation | y=0.875+0.127x | y=0.836+0.094x | y=0.738+0.112x | |
| r | 0.962 | 0.984 | 0.906 | |||
| T1/2/d | 5.45 | 7.37 | 6.18 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.766+0.122x | y=0.852+0.067x | y=0.821+0.101x | ||
| r | 0.947 | 0.978 | 0.969 | |||
| T1/2/d | 5.68 | 10.34 | 6.86 | |||
| 1.5倍剂量 1.5 times the dose | 1次用药 1 dose | 露地 Open field | 降解方程 Degradation equation | y=0.522+0.136x | y=0.476+0.226x | y=0.539+0.166x |
| r | 0.934 | 0.925 | 0.942 | |||
| T1/2/d | 5.09 | 3.06 | 4.17 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.529+0.125x | y=0.519+0.196x | y=0.533+0.133x | ||
| r | 0.958 | 0.913 | 0.961 | |||
| T1/2/d | 4.58 | 3.53 | 5.21 | |||
| 2次用药 2 dose | 露地 Open field | 降解方程 Degradation equation | y=0.571+0.11x | y=0.632+0.063x | y=0.558+0.078x | |
| r | 0.901 | 0.924 | 0.949 | |||
| T1/2/d | 6.30 | 11 | 8.88 | |||
| 大棚 Greenhouse | 降解方程 Degradation equation | y=0.556+0.105x | y=0.566+0.059x | y=0.616+0.069x | ||
| r | 0.922 | 0.947 | 0.933 | |||
| T1/2/d | 6.60 | 11.74 | 10.04 |
| 剂量 Dose | 安全间 隔期 PHI/d | 栽培模式 Cultivation mode | 苯醚甲环唑Difenoconazole | 戊唑醇Tebuconazole | 腈菌唑Myclobutanil | ||||||
|---|---|---|---|---|---|---|---|---|---|---|---|
| CRL/ (mg·kg-1) | NEDI | RQ | CRL/ (mg·kg-1) | NEDI | RQ | CRL/ (mg·kg-1) | NEDI | RQ | |||
| 1.0倍剂量 | 14 | 露地Open field | 0.104 | 0.047 3 | 4.73 | 0.106 | 0.0482 | 1.61 | 0.142 | 0.064 6 | 2.15 |
| 1.0 times | 大棚Greenhouse | 0.114 | 0.051 8 | 5.18 | 0.132 | 0.0601 | 2.01 | 0.124 | 0.056 4 | 1.88 | |
| the dose | 21 | 露地Open field | 0.046 | 0.020 9 | 2.09 | 0.076 | 0.0345 | 1.15 | 0.085 | 0.038 6 | 1.28 |
| 大棚Greenhouse | 0.054 | 0.024 5 | 2.45 | 0.108 | 0.0491 | 1.638 | 0.069 | 0.031 4 | 1.04 | ||
| 28 | 露地Open field | 0.010 | 0.004 6 | 0.455 | 0.0280 | 0.0127 | 0.425 | 0.012 | 0.005 5 | 0.182 | |
| 大棚Greenhouse | 0.011 | 0.005 0 | 0.500 | 0.071 | 0.0323 | 1.076 | 0.022 | 0.0100 | 0.333 | ||
| 1.5倍剂量 | 14 | 露地Open field | 0.142 | 0.064 6 | 6.46 | 0.202 | 0.0919 | 3.06 | 0.186 | 0.0846 | 2.82 |
| 1.5 times | 大棚Greenhouse | 0.165 | 0.075 1 | 7.51 | 0.226 | 0.102 0 | 3.42 | 0.196 | 0.0891 | 2.97 | |
| the dose | 21 | 露地Open field | 0.106 | 0.048 2 | 4.82 | 0.176 | 0.080 0 | 2.67 | 0.136 | 0.0618 | 2.06 |
| 大棚Greenhouse | 0.102 | 0.046 4 | 4.64 | 0.208 | 0.0946 | 3.15 | 0.126 | 0.0573 | 1.91 | ||
| 28 d | 露地Open field | 0.018 | 0.004 9 | 0.491 | 0.088 | 0.0400 | 1.33 | 0.062 | 0.0282 | 0.940 | |
| 大棚Greenhouse | 0.022 | 0.0100 | 1.01 | 0.101 | 0.0459 | 1.53 | 0.086 | 0.0391 | 1.304 | ||
| ADI(mg·kg-1 bw) | 0.01 | 0.03 | 0.03 | ||||||||
Table 5 Residue and risk assessment of three pesticides in broccoli with different PHI
| 剂量 Dose | 安全间 隔期 PHI/d | 栽培模式 Cultivation mode | 苯醚甲环唑Difenoconazole | 戊唑醇Tebuconazole | 腈菌唑Myclobutanil | ||||||
|---|---|---|---|---|---|---|---|---|---|---|---|
| CRL/ (mg·kg-1) | NEDI | RQ | CRL/ (mg·kg-1) | NEDI | RQ | CRL/ (mg·kg-1) | NEDI | RQ | |||
| 1.0倍剂量 | 14 | 露地Open field | 0.104 | 0.047 3 | 4.73 | 0.106 | 0.0482 | 1.61 | 0.142 | 0.064 6 | 2.15 |
| 1.0 times | 大棚Greenhouse | 0.114 | 0.051 8 | 5.18 | 0.132 | 0.0601 | 2.01 | 0.124 | 0.056 4 | 1.88 | |
| the dose | 21 | 露地Open field | 0.046 | 0.020 9 | 2.09 | 0.076 | 0.0345 | 1.15 | 0.085 | 0.038 6 | 1.28 |
| 大棚Greenhouse | 0.054 | 0.024 5 | 2.45 | 0.108 | 0.0491 | 1.638 | 0.069 | 0.031 4 | 1.04 | ||
| 28 | 露地Open field | 0.010 | 0.004 6 | 0.455 | 0.0280 | 0.0127 | 0.425 | 0.012 | 0.005 5 | 0.182 | |
| 大棚Greenhouse | 0.011 | 0.005 0 | 0.500 | 0.071 | 0.0323 | 1.076 | 0.022 | 0.0100 | 0.333 | ||
| 1.5倍剂量 | 14 | 露地Open field | 0.142 | 0.064 6 | 6.46 | 0.202 | 0.0919 | 3.06 | 0.186 | 0.0846 | 2.82 |
| 1.5 times | 大棚Greenhouse | 0.165 | 0.075 1 | 7.51 | 0.226 | 0.102 0 | 3.42 | 0.196 | 0.0891 | 2.97 | |
| the dose | 21 | 露地Open field | 0.106 | 0.048 2 | 4.82 | 0.176 | 0.080 0 | 2.67 | 0.136 | 0.0618 | 2.06 |
| 大棚Greenhouse | 0.102 | 0.046 4 | 4.64 | 0.208 | 0.0946 | 3.15 | 0.126 | 0.0573 | 1.91 | ||
| 28 d | 露地Open field | 0.018 | 0.004 9 | 0.491 | 0.088 | 0.0400 | 1.33 | 0.062 | 0.0282 | 0.940 | |
| 大棚Greenhouse | 0.022 | 0.0100 | 1.01 | 0.101 | 0.0459 | 1.53 | 0.086 | 0.0391 | 1.304 | ||
| ADI(mg·kg-1 bw) | 0.01 | 0.03 | 0.03 | ||||||||
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