Determination of Market, Field Samples, and Dietary Risk Assessment of Chlorfenapyr and Tralopyril in 16 Crops
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Sample Collection
- (1).
- The collection of market samples
- (2).
- Field trials
2.3. Sample Extraction and Purification
2.4. Instrumental Parameters
2.4.1. UHPLC-MS/MS Parameters
2.4.2. GC-MS/MS Parameters
2.5. Method Validation
2.6. Dietary Risk Assessment
3. Results and Discussion
3.1. Optimization of UHPLC-MS/MS and GC-MS/MS
HPLC–MS/MS Optimization Conditions
3.2. Optimization of Sample Pretreatment
3.3. Method Validation
3.4. Residues of Chlorfenapyr and Tralopyril in 16 Market Samples
3.5. Terminal Residues and Dissipation Behaviors of Chlorfenapyr in Cabbage Samples
3.6. Dietary Risk Assessment
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Matrix | Pesticides | (y =) Standard Curve | R2 | ME | LOQ (mg kg−1) | RSDs (n = 5, %) | ||
---|---|---|---|---|---|---|---|---|
Addition Levels (mg kg−1) | ||||||||
0.01 | 1 | 10 (20*) | ||||||
Solvent | Chlorfenapyr | 3,754,158 x − 22,467 | 0.9989 | - | 0.01 | - | - | - |
Tralopyril | 2,421,878 x + 13,065 | 0.9991 | - | 0.01 | - | - | - | |
Chinese cabbage | Chlorfenapyr | 3,660,723 x + 4630 | 0.9993 | 0.98 | 0.01 | 7.4 | 5.0 | 4.7 |
Tralopyril | 2,555,390 x + 16,483 | 0.9989 | 1.06 | 0.01 | 8.0 | 5.9 | 3.7 | |
Welsh onion | Chlorfenapyr | 3,310,947 x + 6823 | 0.9991 | 0.88 | 0.01 | 8.4 | 3.5 | 1.5 |
Tralopyril | 2,445,312 x + 22,932 | 0.9969 | 1.01 | 0.01 | 9.0 | 4.6 | 2.2 | |
Beans | Chlorfenapyr | 3,096,302 x + 3941 | 0.9994 | 0.82 | 0.01 | 7.1 | 3.1 | 4.6 |
Tralopyril | 2,529,608 x + 15,401 | 0.9984 | 1.04 | 0.01 | 10.3 | 6.5 | 2.9 | |
Citrus | Chlorfenapyr | 3,428,831 x − 3229 | 0.9993 | 0.91 | 0.01 | 7.1 | 3.2 | 3.1 |
Tralopyril | 2,305,545 x + 13,773 | 0.9993 | 0.95 | 0.01 | 5.4 | 5.6 | 1.5 | |
Cucumber | Chlorfenapyr | 3,507,036 x + 748 | 0.9996 | 0.93 | 0.01 | 5.2 | 5.7 | 3.4 |
Tralopyril | 2,562,382 x + 7001 | 0.9994 | 1.06 | 0.01 | 7.3 | 3.0 | 3.1 | |
Ginger | Chlorfenapyr | 3,575,404 x + 2848 | 0.9994 | 0.95 | 0.01 | 9.2 | 4.7 | 2.6 |
Tralopyril | 2,370,895 x + 10,212 | 0.9997 | 0.98 | 0.01 | 6.2 | 4.0 | 4.4 | |
Hairy gourd | Chlorfenapyr | 3,798,376 x + 619 | 0.9998 | 1.01 | 0.01 | 9.7 | 3.5 | 2.9 |
Tralopyril | 2,384,714 x + 17,640 | 0.9987 | 0.98 | 0.01 | 3.3 | 2.0 | 4.5 | |
Cabbage mustard | Chlorfenapyr | 3,317,870 x + 13,073 | 0.9993 | 0.88 | 0.01 | 10.0 | 3.1 | 4.0 |
Tralopyril | 2,567,317 x + 11,381 | 0.9992 | 1.06 | 0.01 | 7.1 | 4.1 | 1.7 | |
Leek | Chlorfenapyr | 34,89,748 x + 13,280 | 0.9996 | 0.93 | 0.01 | 11.1 | 4.6 | 3.5 |
Tralopyril | 2,500,523 x − 7439 | 0.9966 | 1.03 | 0.01 | 7.2 | 3.0 | 2.4 | |
Pear | Chlorfenapyr | 3,063,084 x + 18,341 | 0.9999 | 0.82 | 0.01 | 5.2 | 3.8 | 4.5 |
Tralopyril | 2,425,250 x + 12,353 | 0.9993 | 1.00 | 0.01 | 9.1 | 3.4 | 2.4 | |
Eggplant | Chlorfenapyr | 3,409,683 x + 6121 | 0.9996 | 0.91 | 0.01 | 9.7 | 2.7 | 2.4 |
Tralopyril | 2,221,298 x + 21,405 | 0.9976 | 0.92 | 0.01 | 6.1 | 4.8 | 3.3 | |
Pak choi | Chlorfenapyr | 3,275,217 x + 13,699 | 0.9991 | 0.87 | 0.01 | 7.8 | 4.2 | 1.3 |
Tralopyril | 2,379,877 x + 546 | 0.9998 | 0.98 | 0.01 | 7.4 | 3.4 | 1.4 | |
Cowpea | Chlorfenapyr | 3,015,524 x + 28,920 | 0.9994 | 0.80 | 0.01 | 6.9 | 5.6 | 2.5 |
Tralopyril | 2,555,844 x + 9531 | 0.9995 | 1.06 | 0.01 | 8.9 | 4.2 | 5.4 | |
Cabbage | Chlorfenapyr | 3,547,825 x − 5212 | 0.9991 | 0.95 | 0.01 | 6.3 | 6.2 | 2 |
Tralopyril | 2,458,083 x + 12,693 | 0.9992 | 1.01 | 0.01 | 3.6 | 1.7 | 1.9 | |
Apple | Chlorfenapyr | 3,653,855 x + 8117 | 0.9999 | 0.97 | 0.01 | 4.6 | 2.6 | 2.7 |
Tralopyril | 2,400,056 x + 13,172 | 0.9992 | 0.99 | 0.01 | 3.1 | 1.5 | 2 | |
Tea | Chlorfenapyr | 3,486,223 x − 7105 | 0.9991 | 0.93 | 0.01 | 6.2 | 7 | 2.2 |
Tralopyril | 2,395,137 x + 9500 | 0.9996 | 0.99 | 0.01 | 4.1 | 1.7 | 2.6 |
Sampling Locations | Market Type | Matrix | Chlorfenapyr | Tralopyril | ||
---|---|---|---|---|---|---|
Detection Quantity (mg kg−1) | Exceed Standard | Detection Quantity (mg kg−1) | Exceed Standard | |||
Yabo RT-Mart | Supermarket | Chinese cabbage | 0.112 | No | — | — |
cowpea | 0.404 | unset limits | 0.01 | unset limits | ||
leek | 0.022 | unset limits | — | — | ||
Tesco Lifestyle | Minimarket | beans | 0.048 | unset limits | — | — |
eggplant | 0.099 | No | — | — | ||
leek | 0.224 | unset limits | — | — | ||
RT-Mart | Supermarket | eggplant | 0.192 | No | — | — |
cowpea | 0.019 | unset limits | — | — | ||
New Age Supermarket | Supermarket | beans | 0.042 | unset limits | — | — |
cucumber | 0.225 | No | — | — | ||
Jiayue Supermarket | Supermarket | cabbage | 0.104 | No | — | — |
leek | 0.054 | unset limits | — | — | ||
Four Seasons Supermarket | Minimarket | cabbage mustard | 0.023 | No | — | — |
leek | 0.262 | unset limits | — | — | ||
pak choi | 0.281 | No | — | — | ||
tea | 0.111 | unset limits | — | — | ||
Provincial Farmer’s Market | Farmer’s market | cucumber | 0.017 | No | — | — |
cowpea | 0.024 | unset limits | — | — | ||
tea | 0.021 | No | — | — | ||
Wide Supermarket | Minimarket | eggplant | 0.050 | No | — | — |
cabbage mustard | 0.014 | No | — | — | ||
pak choi | 0.014 | No | — | — | ||
Lattice Supermarket | Supermarket | cowpea | 0.172 | unset limits | — | — |
cabbage mustard | 0.462 | Yes | — | — | ||
pak choi | 0.025 | No | — | — | ||
Wuma Farmer’s Wholesale Market | Farmer’s market | cucumber | 0.246 | No | — | — |
tea | 0.024 | unset limits | — | — | ||
Yingsheng Farmer’s Market | Farmer’s market | leek | 0.056 | unset limits | — | — |
C ‘mon Lotus Supermarket | Supermarket | tea | 0.092 | unset limits | — | — |
Zaohang Farmer’s Wholesale Market | Farmer’s market | eggplant | 0.027 | No | — | — |
cowpea | 0.024 | unset limits | — | — | ||
Rundu Supermarket | Minimarket | beans | 0.036 | unset limits | — | — |
cabbage | 0.015 | No | — | — | ||
cucumber | 0.044 | unset limits | — | — | ||
leek | 0.026 | unset limits | — | — | ||
tea | 0.019 | No | — | — | ||
Baibayu Convenient Market | Farmer’s market | beans | 0.041 | unset limits | — | — |
leek | 0.182 | unset limits | — | — |
Test Site | Application Dose (g ha−1) | Application Times (Freq) | Harvest Interval (Days) | Residual Quantity (mg kg−1) | STMR (mg kg−1) | HR (mg kg−1) |
---|---|---|---|---|---|---|
Liaoning, Shanxi, Beijing, Shandong, Shanghai, Anhui, Hunan, Jiangxi, Guangxi, Chongqing, Guizhou, Guangdong | 120 | 2 | 14 | <0.01, 0.015, 0.016, 0.067, 0.070, 0.089, 0.121, 0.210, 0.213, 0.310, 0.337, 0.471 | 0.105 | 0.471 |
21 | <0.01 (8), 0.014, 0.031, 0.046, 0.144 | 0.01 | 0.144 |
Pesticide | Food Types | Intake (kg) | Residue (mg kg−1) | Sources of Residues | NEDI (mg) | Daily Intake Allowed (mg) | Risk Probability |
---|---|---|---|---|---|---|---|
Chlorfenapyr (no consideration of tralopyril) | Dark vegetables | 0.0915 | 10 | Residue limit (pak choi) | 0.915 | ADI × 63 | NEDI/(ADI × 63) |
Light vegetables | 0.1837 | 0.404 | Market monitoring (cowpea) | 0.074 | |||
Fruits | 0.0457 | 0.54 | Residue limit (mulberry) | 0.025 | |||
Salt | 0.012 | 20 | Residue limit (tea) | 0.240 | |||
Soy sauce | 0.009 | 0.111 | Market monitoring (ginger) | 0.001 | |||
Sum | 1.0286 | 1.255 | 1.929 | 65.1 % | |||
Chlorfenapyr (consideration of tralopyril) | Food types | Intake (kg) | Residue (mg kg−1) | Sources of residues | NEDI (mg) | Daily intake allowed (mg) | Risk probability |
Dark vegetables | 0.0915 | 10 | Residue limit (pak choi) | 0.915 | ADI × 63 | NEDI/(ADI × 63) | |
Light vegetables | 0.1837 | 0.504 | Market monitoring (cowpea) | 0.093 | |||
Fruits | 0.0457 | 0.54 | Residue limit (mulberry) | 0.025 | |||
Salt | 0.012 | 20 | Residue limit (tea) | 0.240 | |||
Soy sauce | 0.009 | 0.111 | Market monitoring (ginger) | 0.001 | |||
Sum | 1.0286 | 1.274 | 1.929 | 66.0% |
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Li, H.; Sun, F.; Hu, S.; Sun, Q.; Zou, N.; Li, B.; Mu, W.; Lin, J. Determination of Market, Field Samples, and Dietary Risk Assessment of Chlorfenapyr and Tralopyril in 16 Crops. Foods 2022, 11, 1246. https://0-doi-org.brum.beds.ac.uk/10.3390/foods11091246
Li H, Sun F, Hu S, Sun Q, Zou N, Li B, Mu W, Lin J. Determination of Market, Field Samples, and Dietary Risk Assessment of Chlorfenapyr and Tralopyril in 16 Crops. Foods. 2022; 11(9):1246. https://0-doi-org.brum.beds.ac.uk/10.3390/foods11091246
Chicago/Turabian StyleLi, Hong, Fengshou Sun, Shuai Hu, Qi Sun, Nan Zou, Beixing Li, Wei Mu, and Jin Lin. 2022. "Determination of Market, Field Samples, and Dietary Risk Assessment of Chlorfenapyr and Tralopyril in 16 Crops" Foods 11, no. 9: 1246. https://0-doi-org.brum.beds.ac.uk/10.3390/foods11091246