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Peaks | tR (min) | Polarity | Precursor Ion | Product Ion | Transition Type | |
---|---|---|---|---|---|---|
1. | Atrazine-d5 | 4.57 | Positive | 220.0 | 58.0 | Quantifier |
2. | Atrazine-d5 | 4.57 | Positive | 205.0 | 127.0 | Qualifier |
3. | Quintozene | 4.70 | Positive | 294.9 | 236.9 | Quantifier |
4. | Quintozene | 4.70 | Positive | 236.8 | 118.9 | Qualifier |
5. | Methyl parathion | 4.96 | Positive | 263.0 | 109.0 | Quantifier |
6. | Methyl parathion | 4.96 | Positive | 263.0 | 79.0 | Qualifier |
7. | Captan | 5.47 | Positive | 184.0 | 149.1 | Quantifier |
8. | Captan | 5.47 | Positive | 184.0 | 134.1 | Qualifier |
9. | trans-Chlordane | 5.48 | Positive | 271.9 | 237.0 | Quantifier |
10. | trans-Chlordane | 5.48 | Positive | 372.9 | 265.9 | Qualifier |
11. | cis-Chlordane | 5.56 | Positive | 372.9 | 265.9 | Quantifier |
12. | cis-Chlordane | 5.56 | Positive | 271.9 | 237.0 | Qualifier |
13. | Chlorfenapyr | 5.69 | Positive | 247.1 | 227.1 | Quantifier |
14. | Chlorfenapyr | 5.69 | Positive | 59.1 | 31.1 | Qualifier |
15. | Cyfluthrin | 6.71 | Positive | 226.0 | 206.0 | Quantifier |
16. | Cyfluthrin | 6.71 | Positive | 163.0 | 127.0 | Qualifier |
17. | Cypermethrin | 6.80 | Positive | 163.0 | 127.1 | Quantifier |
18. | Cypermethrin | 6.80 | Positive | 181.1 | 152.1 | Qualifier |
Column | Low-pressure GC column kit (factory-coupled restrictor column [5 m x 0.18 mm ID] and Rtx-5ms analytical column [15 m, 0.53 mm ID, 1 µm plus 1 m integrated transfer line on the outlet end]) (cat.# 11800) |
---|---|
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) | |
Diluent: | Acetonitrile |
Conc.: | 5.8-8.4 ng/mL Expected concentration range (70-100% recovery) in extract after extracting from chocolate fortified at 100 ng/g (final extract was diluted in half with acidified 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.: | 80 °C (hold 1 min) to 330 °C at 45 °C/min (hold 5.5 min) |
Carrier Gas | He, constant flow |
Flow Rate: | 2.0 mL/min |
Detector | MS/MS |
---|---|
Transfer Line Temp.: | 290 °C |
Analyzer Type: | Quadrupole |
Source Temp.: | 325 °C |
Electron Energy: | 70 eV |
Tune Type: | PFTBA |
Ionization Mode: | EI |
Instrument | Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS |
Sample Preparation | Chocolate was pulverized using a SPEX Freezer/Mill grinder, and 0.5 g sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. Then, 0.5 mL of isopropyl alcohol was added to the sample. The sample was vortexed for 10 sec or until a homogenous mixture was obtained. Afterwards, 2.5 mL of acetonitrile acidified with acetic acid at 1% v/v was added to the vial. Once again, the mixture was vortexed for 30 sec, and then centrifuged for 5 min at 4300 ×g at room temperature. A total of 2 mL of the supernatant was passed through 100 mg Resprep C18 SPE cartridge (cat.# 26030). 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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