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Peaks | tR (min) | Polarity | Precursor Ion | Product Ion | Transition Type | |
---|---|---|---|---|---|---|
1. | Atrazine-d5 | 6.82 | Positive | 220.0 | 58.0 | Quantifier |
2. | Atrazine-d5 | 6.82 | Positive | 205.0 | 127.0 | Qualifier |
3. | Diazinon-d10 (diethyl-d10) | 7.01 | Positive | 183.0 | 139.0 | Quantifier |
4. | Diazinon-d10 (diethyl-d10) | 7.01 | Positive | 183.0 | 168.0 | Qualifier |
5. | Quintozene | 7.03 | Positive | 294.9 | 236.9 | Quantifier |
6. | Quintozene | 7.03 | Positive | 236.8 | 118.9 | Qualifier |
7. | Methyl parathion | 7.50 | Positive | 263.0 | 109.0 | Quantifier |
8. | Methyl parathion | 7.50 | Positive | 263.0 | 79.0 | Qualifier |
9. | Captan | 8.37 | Positive | 184.0 | 149.1 | Quantifier |
10. | Captan | 8.37 | Positive | 184.0 | 134.1 | Qualifier |
11. | trans-Chlordane | 8.41 | Positive | 271.9 | 237.0 | Quantifier |
12. | trans-Chlordane | 8.41 | Positive | 372.9 | 265.9 | Qualifier |
13. | cis-Chlordane | 8.53 | Positive | 372.9 | 265.9 | Quantifier |
14. | cis-Chlordane | 8.53 | Positive | 271.9 | 237.0 | Qualifier |
15. | Chlorfenapyr | 8.80 | Positive | 247.1 | 227.1 | Quantifier |
16. | Chlorfenapyr | 8.80 | Positive | 59.1 | 31.1 | Qualifier |
17. | Cyfluthrin | 10.61 | Positive | 226.0 | 206.0 | Quantifier |
18. | Cyfluthrin | 10.61 | Positive | 163.0 | 127.0 | Qualifier |
19. | Cypermethrin | 10.87 | Positive | 163.0 | 127.1 | Quantifier |
20. | Cypermethrin | 10.87 | Positive | 181.1 | 152.1 | Qualifier |
Column | Rxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423) |
---|---|
Standard/Sample | California pesticide standard #1 (cat.# 34124) |
California pesticide standard #2 (cat.# 34125) | |
California pesticide standard #3 (cat.# 34126) | |
California pesticide standard #4 (cat.# 34127) | |
California pesticide standard #5 (cat.# 34128) | |
California pesticide standard #6 (cat.# 34129) | |
Atrazine-d5 (cat.# 31984) | |
Diazinon-d10 (cat.# 31986) | |
Diluent: | Acetonitrile |
Conc.: | 2.5-10 ng/mL Expected concentration range in extract after extracting from gummy fortified at 100 ng/g (final extract was diluted in half with acetonitrile). |
Injection | |
Inj. Vol.: | 1 µL splitless |
Liner: | Topaz 4.0 mm ID single taper inlet liner w/wool (cat.# 23447) |
Inj. Temp.: | 250 °C |
Purge Flow: | 5 mL/min |
Oven | |
Oven Temp.: | 90 °C (hold 1 min) to 310 °C at 25 °C/min (hold 10 min) |
Carrier Gas | He, constant flow |
Flow Rate: | 1.4 mL/min |
Detector | MS/MS |
---|---|
Transfer Line Temp.: | 290 °C |
Analyzer Type: | Quadrupole |
Source Temp.: | 330 °C |
Electron Energy: | 70 eV |
Tune Type: | PFTBA |
Ionization Mode: | EI |
Instrument | Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS |
Sample Preparation | Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 1.9 mL of supernatant was transferred to a Q-sep QuEChERS dSPE tube containing pre-weighed magnesium sulfate, PSA, and GCB (cat.# 26217). After vortexing and centrifuging, 500 μL of extract was mixed with 500 μL of acidified acetonitrile. 1 μL of final extract was injected into the GC-MS/MS system. |
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