A Green Bridge: Enhancing a Multi-Pesticide Test for Food by Phase-Transfer Sample Treatment Coupled with LC/MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Selection of Food Substrates and Target Substances
2.2. Optimization of LC–MS/MS Conditions
2.3. Optimization of Pre-Treatment Methods
2.3.1. Optimization of Pre-Treatment Method 1
Selection of Purification Materials
Choice of Carrageenan Quantity
2.3.2. Optimization of Pre-Treatment Method 2
2.4. Matrix Effect
2.5. Methodological Evaluation
2.5.1. Standard Curve and Detection Limit
2.5.2. Precision and Recovery Rate
2.6. Determination of Actual Samples
3. Materials and Methods
3.1. Instruments and Reagents
3.2. Sample Pretreatment Method
3.3. LC–MS/MS Conditions
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Pesticides | Relative Retention Time ** | Transitions (m/z) | Dewell Time (mS) | Fragmentor (V) | CE (eV) |
---|---|---|---|---|---|
aminocarb | 0.06 | 209.3/152.1 *, 209.3/137.1 | 100 | 70 | 9, 25 |
propamocarb | 0.06 | 189.2/102.1 *, 189.2/144.1 | 100 | 70 | 13, 9 |
aldicarb sulfoxide | 0.11 | 229.1/166.1 *, 229.1/109.1 | 60 | 70 | 5, 13 |
aldicarb sulfone | 0.13 | 245.1/166.1 *, 245.1/109.1 | 60 | 60 | 13, 17 |
oxamyl | 0.13 | 242.1/72.1 *, 242.1/121.2 | 60 | 55 | 17, 9 |
thiofanox sulfoxide | 0.26 | 257.1/200.0 *, 257.1/137.2 | 40 | 65 | 5, 13 |
pirimicarb | 0.31 | 239.3/72.1 *, 239.3/182.1 | 40 | 65 | 20, 13 |
thiofanox sulfone | 0.31 | 273.1/216.1 *, 273.1/137.1 | 40 | 65 | 9, 21 |
3-hydroxycarbofuran | 0.38 | 238.4/163.1 *, 238.4/181.1 | 40 | 100 | 9, 5 |
dioxacarb | 0.38 | 224.2/167.1 *, 224.2/123.1 | 40 | 40 | 5, 13 |
aldicarb | 0.63 | 213.1/89.1 *, 213.1/116.1 | 200 | 75 | 13, 9 |
metolcarb | 0.73 | 166.2/109.1 *, 166.2/94.1 | 200 | 30 | 9, 35 |
propoxur | 0.82 | 210.2/111.0 *, 210.2/168.3 | 60 | 30 | 9, 4 |
carbofuran | 0.85 | 222.3/165.1 *, 222.3/123.1 | 60 | 70 | 9, 21 |
bendiocarb | 0.85 | 224.1/167.1 *, 224.1/109.1 | 60 | 70 | 5, 17 |
carbaryl | 0.95 | 202.1/145.0 *, 202.1/127.3 | 60 | 40 | 5, 33 |
ethiofencarb | 1.00 | 226.1/107.1 *, 226.1/164.1 | 60 | 50 | 5, 9 |
thiofanox | 1.02 | 241.1/184.1 *, 241.1/57.2 | 60 | 60 | 5, 17 |
thiocarb | 1.06 | 377.0/64.1 *, 377.0/113.0 | 60 | 120 | 13, 9 |
isoproarb | 1.13 | 194.1/137.1 *, 194.1/95.1 | 60 | 60 | 5, 9 |
2,3,5-trimethacarb | 1.13 | 137.1/122.0 *, 137.1/107.2 | 60 | 130 | 17, 25 |
fenobucarb | 1.27 | 208.1/95.1 *, 208.1/152.1 | 40 | 60 | 9, 4 |
diethofencarb | 1.29 | 268.2/226.1 *, 268.2/152.2 | 40 | 55 | 21, 5 |
methiocarb | 1.31 | 226.1/169.1 *, 226.1/121.1 | 40 | 55 | 5, 17 |
promecarb | 1.33 | 208.1/109.1 *, 208.1/105.1 | 40 | 50 | 5, 13 |
fenoxycarb | 1.53 | 302.3/88.1 *, 302.3/116.1 | 100 | 100 | 17, 5 |
indoxacarb | 1.70 | 528.1/150.2 *, 528.1/293.2 | 100 | 150 | 21, 9 |
benfuracarb | 1.75 | 411.2/195.0 *, 411.2/252.1 | 100 | 90 | 21, 9 |
furathiocarb | 1.80 | 383.2/252.1 *, 383.2/167.1 | 100 | 90 | 5, 25 |
carbosuifan | 2.06 | 381.6/118.1 *, 381.6/160.1 | 200 | 130 | 13, 9 |
Substrates | Pesticide | Carrageenan Addition/g in 20 mL | ||||
---|---|---|---|---|---|---|
0.3 | 0.5 | 0.7 | 0.9 | 1.1 | ||
Banana | Oxamyl | 95.2 | 97.6 | 97.1 | 96.3 | 95.9 |
Ethiofencarb | 94.2 | 96.1 | 96.3 | 95.4 | 95.4 | |
Lemon | Oxamyl | 95.3 | 97.4 | 97.1 | 97.1 | 96.5 |
Ethiofencarb | 96.4 | 98.2 | 97.7 | 97.5 | 96.4 | |
Apple | Oxamyl | 95.4 | 97.5 | 97.2 | 97.1 | 96.5 |
Ethiofencarb | 94.3 | 98 | 97.9 | 96.4 | 96.2 | |
Spinach | Oxamyl | 91.4 | 94 | 94.1 | 95.2 | 96.3 |
Ethiofencarb | 92 | 93.1 | 95.7 | 96.4 | 96.8 | |
Cabbage | Oxamyl | 96.7 | 98.2 | 98 | 97.4 | 97.1 |
Ethiofencarb | 95.7 | 97.8 | 97.1 | 96.4 | 96.4 | |
Rice | Oxamyl | 97.9 | 97.2 | 96.5 | 96.5 | 95.9 |
Ethiofencarb | 98.1 | 97.2 | 97.1 | 96.8 | 96.1 |
Pesticide | Banana | Lemon | Apple | Spinach | Cabbage | Rice | ||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
M1 * | M2 ** | M1 * | M2 ** | M1 * | M2 ** | M1 * | M2 ** | M1 * | M2 ** | M1 * | M2 ** | |
aminocarb | 0.8 | 0.6 | 0.7 | 0.3 | 0.8 | 0.7 | 0.7 | 0.5 | 0.8 | 0.7 | 0.9 | 0.9 |
propamocarb | 1.1 | 0.9 | 0.8 | 0.7 | 0.9 | 0.9 | 0.8 | 0.7 | 0.9 | 0.9 | 0.8 | 0.8 |
aldicarb sulfoxide | 1.1 | 1.1 | 0.9 | 0.7 | 0.9 | 1.1 | 0.7 | 0.7 | 0.8 | 0.7 | 0.9 | 0.9 |
aldicarb sulfone | 1.1 | 1.1 | 0.9 | 0.8 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.9 | 0.9 |
oxamyl | 1.1 | 1.1 | 0.9 | 0.9 | 0.9 | 0.9 | 0.7 | 0.7 | 0.9 | 0.9 | 0.9 | 0.9 |
thiofanox sulfoxide | 1.1 | 1.1 | 0.9 | 0.8 | 0.9 | 0.9 | 0.7 | 0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
pirimicarb | 1.1 | 1.2 | 0.8 | 0.6 | 0.9 | 0.9 | 0.8 | 0.7 | 0.9 | 0.9 | 0.9 | 0.9 |
thiofanox sulfone | 1.1 | 1.1 | 0.8 | 0.7 | 0.9 | 0.9 | 0.8 | 0.7 | 0.9 | 0.9 | 0.9 | 0.9 |
3-hydroxycarbofuran | 1.1 | 1.1 | 0.9 | 0.8 | 0.9 | 0.9 | 0.8 | 0.7 | 0.7 | 0.6 | 0.9 | 0.9 |
dioxacarb | 1.1 | 1.1 | 0.7 | 0.7 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.8 | 0.8 |
aldicarb | 1.1 | 1.1 | 0.9 | 0.8 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.8 | 0.6 |
metolcarb | 1.1 | 1.1 | 0.8 | 0.8 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.9 | 0.9 |
propoxur | 1.1 | 1.1 | 0.8 | 0.7 | 0.9 | 0.9 | 0.8 | 0.5 | 0.9 | 0.9 | 0.9 | 0.9 |
carbofuran | 1.1 | 1.2 | 0.8 | 0.7 | 0.9 | 0.9 | 0.7 | 0.5 | 0.9 | 0.9 | 0.7 | 0.7 |
bendiocarb | 1.1 | 1.1 | 0.8 | 0.8 | 0.9 | 0.9 | 0.7 | 0.5 | 0.9 | 0.9 | 0.8 | 0.8 |
carbaryl | 1.1 | 1.2 | 0.8 | 0.9 | 0.9 | 0.9 | 0.7 | 0.5 | 0.9 | 0.9 | 0.8 | 0.8 |
ethiofencarb | 1.1 | 1.1 | 0.8 | 0.7 | 0.9 | 0.9 | 0.7 | 0.4 | 0.9 | 0.9 | 0.8 | 0.7 |
thiofanox | 1.1 | 1.2 | 0.8 | 0.7 | 0.9 | 0.9 | 0.6 | 0.5 | 0.9 | 0.9 | 0.7 | 0.7 |
thiocarb | 1.2 | 1.3 | 0.9 | 0.8 | 0.9 | 0.8 | 0.8 | 0.8 | 0.9 | 0.9 | 0.9 | 0.9 |
isoproarb | 1.1 | 1.1 | 0.8 | 0.8 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.9 | 0.9 |
2,3,5-trimethacarb | 0.9 | 1.1 | 0.8 | 0.6 | 0.9 | 0.8 | 0.7 | 0.6 | 0.9 | 0.9 | 0.7 | 0.7 |
fenobucarb | 1.1 | 1.1 | 0.7 | 0.5 | 0.8 | 0.8 | 0.5 | 0.3 | 0.7 | 0.6 | 0.8 | 0.6 |
diethofencarb | 1.1 | 1.1 | 0.9 | 0.7 | 0.9 | 0.9 | 0.9 | 0.9 | 0.8 | 0.6 | 0.8 | 0.8 |
methiocarb | 1.1 | 1.1 | 0.9 | 0.7 | 0.9 | 0.9 | 0.5 | 0.3 | 0.7 | 0.7 | 0.8 | 0.8 |
promecarb | 1.1 | 1.1 | 0.8 | 0.7 | 0.9 | 0.9 | 0.6 | 0.4 | 0.7 | 0.7 | 0.9 | 0.9 |
fenoxycarb | 1.1 | 1.1 | 0.8 | 0.7 | 0.9 | 0.9 | 0.6 | 0.3 | 0.9 | 0.9 | 0.8 | 0.8 |
indoxacarb | 1.1 | 0.9 | 1.1 | 1.2 | 0.9 | 0.9 | 0.6 | 0.5 | 0.9 | 0.9 | 0.7 | 0.6 |
benfuracarb | 1.1 | 0.9 | 0.9 | 0.7 | 0.9 | 0.9 | 0.8 | 0.7 | 0.7 | 0.6 | 0.6 | 0.5 |
furathiocarb | 0.9 | 0.9 | 0.8 | 0.8 | 0.9 | 0.9 | 0.7 | 0.6 | 0.9 | 0.9 | 0.8 | 0.8 |
carbosuifan | 0.9 | 0.9 | 0.8 | 0.6 | 0.9 | 0.9 | 0.7 | 0.6 | 0.8 | 0.8 | 0.9 | 0.9 |
Pesticide | Rate of Linear Slope | Rate of Intercept | Comparison of Recovery | ||
---|---|---|---|---|---|
5 µg/kg | 20 µg/kg | 100 µg/kg | |||
aminocarb | 1.2 | 0.5 | 1.05 | 1.01 | 1.03 |
propamocarb | 1.1 | 0.4 | 1.04 | 1.04 | 1.01 |
aldicarb sulfoxide | 1.2 | 0.5 | 1.05 | 1.03 | 1.01 |
aldicarb sulfone | 1.2 | 0.3 | 1.03 | 1.08 | 1.02 |
oxamyl | 1.1 | 0.6 | 1.06 | 1.01 | 1.02 |
thiofanox sulfoxide | 1.1 | 0.7 | 1.07 | 1.03 | 1.03 |
pirimicarb | 1.3 | 0.5 | 1.05 | 1.05 | 1.04 |
thiofanox sulfone | 1.2 | 0.4 | 1.04 | 1.02 | 1.01 |
3-hydroxycarbofuran | 1.1 | 0.4 | 1.04 | 1.03 | 1.02 |
dioxacarb | 1.2 | 0.3 | 1.03 | 1.04 | 1.01 |
aldicarb | 1.1 | 0.4 | 1.04 | 1.01 | 1.01 |
metolcarb | 1.1 | 0.3 | 1.03 | 1.02 | 1.07 |
propoxur | 1.2 | 0.3 | 1.03 | 1.02 | 1.05 |
carbofuran | 1.3 | 0.3 | 1.03 | 1.06 | 1.01 |
bendiocarb | 1.2 | 0.4 | 1.02 | 1.04 | 1.01 |
carbaryl | 1.2 | 0.5 | 1.04 | 1.05 | 1.04 |
ethiofencarb | 1.2 | 0.3 | 1.03 | 1.02 | 1.01 |
thiofanox | 1.2 | 0.3 | 1.03 | 1.01 | 1.06 |
thiocarb | 1.1 | 0.4 | 1.02 | 1.04 | 1.01 |
isoproarb | 1 | 0.2 | 1.02 | 1.02 | 1.04 |
2,3,5-trimethacarb | 1 | 0.2 | 1.02 | 1.03 | 1.05 |
fenobucarb | 1.1 | 0.4 | 1.04 | 1.01 | 1.02 |
diethofencarb | 1.2 | 0.3 | 1.03 | 1.01 | 1.01 |
methiocarb | 1.1 | 0.3 | 1.03 | 1.04 | 1.03 |
promecarb | 1.2 | 0.3 | 1.03 | 1.02 | 1.04 |
fenoxycarb | 1.1 | 0.3 | 1.03 | 1.01 | 1.01 |
indoxacarb | 1.1 | 0.5 | 1.05 | 1.04 | 1.05 |
benfuracarb | 1.1 | 0.5 | 1.05 | 1.03 | 1.02 |
furathiocarb | 1.3 | 0.5 | 1.05 | 1.01 | 1.01 |
carbosuifan | 1.2 | 0.5 | 1.05 | 1.03 | 1.03 |
Matrix | Supplemental Level | RSD Range | ||
---|---|---|---|---|
5 μg/kg | 20 μg/kg | 100 μg/kg | ||
banana | 59.84–127.06% | 60.08–114.06% | 56.13–110.05% | 1.1–15% |
lemon | 62.05–91.61% | 69.33–98.94% | 71.83–107.02% | 0.47–9.3% |
apple | 74.78–106.3% | 60.51–125.2% | 75.40–117.6%, | 3.1–16% |
cabbage | 68.62–103.0% | 69.81–99.31% | 67.62–112.3% | 1.2–13% |
spinach | 71.11–115.3% | 77.45–125.3% | 57.36–103.2% | 3.2–14% |
rice | 85.70–106.0% | 67.31–108.3% | 70.70–97.61% | 0.70–8.5% |
Pesticide | IUPAC Name | Formula |
---|---|---|
aminocarb | [4-(dimethylamino)-3-methylphenyl] N-methylcarbamate | C11H16N2O2 |
propamocarb | propyl N-[3-(dimethylamino)propyl]carbamate | C9H20N2O2 |
aldicarb sulfoxide | [(E)-(2-methyl-2-methylsulfinylpropylidene)amino] N-methylcarbamate | C7H14N2O3S |
aldicarb sulfone | [(E)-(2-methyl-2-methylsulfonylpropylidene)amino] N-methylcarbamate | C7H14N2O4S |
oxamyl | methyl (1Z)-2-(dimethylamino)-N-(methylcarbamoyloxy)-2-oxoethanimidothioate | C7H13N3O3S |
thiofanox sulfoxide | [(Z)-(3,3-dimethyl-1-methylsulfinylbutan-2-ylidene)amino] N-methylcarbamate | C9H18N2O3S |
pirimicarb | [2-(dimethylamino)-5,6-dimethylpyrimidin-4-yl] N,N-dimethylcarbamate | C11H18N4O2 |
thiofanox sulfone | [(3,3-dimethyl-1-methylsulfonylbutan-2-ylidene)amino] N-methylcarbamate | C9H18N2O4S |
3-hydroxycarbofuran | (3-hydroxy-2,2-dimethyl-3H-1-benzofuran-7-yl) N-methylcarbamate | C12H15NO4 |
dioxacarb | [2-(1,3-dioxolan-2-yl)phenyl] N-methylcarbamate | C11H13NO4 |
aldicarb | [(E)-(2-methyl-2-methylsulfonylpropylidene)amino] N-methylcarbamate | C7H14N2O4S |
metolcarb | (3-methylphenyl) N-methylcarbamate | C9H11NO2 |
propoxur | (2-propan-2-yloxyphenyl) N-methylcarbamate | C11H15NO3 |
carbofuran | (2,2-dimethyl-3H-1-benzofuran-7-yl) N-methylcarbamate | C12H15NO3 |
bendiocarb | (2,2-dimethyl-1,3-benzodioxol-4-yl) N-methylcarbamate | C11H13NO4 |
carbaryl | naphthalen-1-yl N-methylcarbamate | C12H11NO2 |
ethiofencarb | [2-(ethylsulfanylmethyl)phenyl] N-methylcarbamate | C11H15NO2S |
thiofanox | [(3,3-dimethyl-1-methylsulfanylbutan-2-ylidene)amino] N-methylcarbamate | C9H18N2O2S |
thiocarb | N,N-diethylcarbamodithioate | C5H16NNaO3S2 |
isoproarb | (2-propan-2-ylphenyl) N-methylcarbamate | C11H15NO2 |
2,3,5-trimethacarb | (2,3,5-trimethylphenyl) N-methylcarbamate | C11H15NO2 |
fenobucarb | (2-butan-2-ylphenyl) N-methylcarbamate | C12H17NO2 |
diethofencarb | propan-2-yl N-(3,4-diethoxyphenyl)carbamate | C14H21NO4 |
methiocarb | (3,5-dimethyl-4-methylsulfanylphenyl) N-methylcarbamate | C11H15NO2S |
promecarb | (3-methyl-5-propan-2-ylphenyl) N-methylcarbamate | C11H15NO2S |
fenoxycarb | ethyl N-[2-(4-phenoxyphenoxy)ethyl]carbamate | C17H19NO4 |
indoxacarb | methyl 7-chloro-2-[methoxycarbonyl-[4-(trifluoromethoxy)phenyl]carbamoyl]-3,5-dihydroindeno [1,2-e][1,3,4]oxadiazine-4a-carboxylate | C22H17ClF3N3O7 |
benfuracarb | ethyl 3-[[(2,2-dimethyl-3H-1-benzofuran-7-yl)oxycarbonyl-methylamino]sulfanyl-propan-2-ylamino]propanoate | C20H30N2O5S |
furathiocarb | (2,2-dimethyl-3H-1-benzofuran-7-yl) N-[butoxycarbonyl(methyl)amino]sulfanyl-N-methylcarbamate | C18H26N2O5S |
carbosuifan | (2,2-dimethyl-3H-1-benzofuran-7-yl) N-(dibutylamino)sulfanyl-N-methylcarbamate | C20H32N2O3S |
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Jin, S.; Shen, Y.; Liu, T.; Liang, R.; Ning, X.; Cao, J. A Green Bridge: Enhancing a Multi-Pesticide Test for Food by Phase-Transfer Sample Treatment Coupled with LC/MS. Molecules 2023, 28, 6756. https://doi.org/10.3390/molecules28196756
Jin S, Shen Y, Liu T, Liang R, Ning X, Cao J. A Green Bridge: Enhancing a Multi-Pesticide Test for Food by Phase-Transfer Sample Treatment Coupled with LC/MS. Molecules. 2023; 28(19):6756. https://doi.org/10.3390/molecules28196756
Chicago/Turabian StyleJin, Shaoming, Yi Shen, Tongtong Liu, Ruiqiang Liang, Xiao Ning, and Jin Cao. 2023. "A Green Bridge: Enhancing a Multi-Pesticide Test for Food by Phase-Transfer Sample Treatment Coupled with LC/MS" Molecules 28, no. 19: 6756. https://doi.org/10.3390/molecules28196756