108139-1 Study Title Data Requirements Author Study ... - IR-4 Project

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Bayer Corporation <strong>108139</strong>-1 Agriculture Division 8. Concentrate the sample to dryness using a turbo-vap (water bath 40 ± 5 °C). 9. Add 2.5 mL of toluene to the 60-mL I-Chem vial and mix thoroughly. 10. Proceed to the final extract preparation for analysis 3.4.3.5 Final Extract Preparation for Analysis 1. To complete the preparation for instrumental analysis, the extract is to be added to a GC vial. 3.4.4 Analysis By Gas Chromatography/Mass Spectrometry (GC/MS) A. GC conditions: Column: DB-5MS capillary column, 5% phenyl methyl, 12 m length, 0.2 mm ID, 0.33- P ILOP WKLFNQHVV DOO PDWULFHV H[FHSW DSSOH DQG SHDU Column: HP-5 capillary column, 5% phenyl methyl, 12 m length, 0.2 mm ID, 0.33- P ILOP WKLFNQHVV DSSOH DQG SHDU Injector port temp: 280 °C (all matrices except apple and pear) 250 °C (apple and pear) Flow: 1 mL/min Mode: Splitless then split at 1.0 min Gas type: Helium Initial oven temp: 150 °C Initial time: 4 min Ramps: 30 °C to a final temp of 300 °C and hold for 11 min Total run time: 20.0 min Approx. Retention Time: 9.4 min B. Mass spectrometer conditions: Ionization mode: negative chemical ionization (NCI) Ionization gas: methane Acquisition mode: Single interaction monitoring (SIM) Solvent delay: 4 min Ion masses: cyfluthrin m/z 207 [ 2 H6]cyfluthrin m/z 213 MS quad temp: 106 °C MS source temp: 150 °C MSD transfer line temp: 300 °C 36
Bayer Corporation <strong>108139</strong>-1 Agriculture Division C. Procedure: 1. Use the chemstation software to run the automated autotune for NCI. 2. Add an aliquot of the final extract or an aliquot of the 0.050 ppm quantification standard (0.050 ppm cyfluthrin and 0.050 ppm [ 2 H6]cyfluthrin) solution in toluene into a GC auto sampler vial. 3. Inject 1 / IURP WKH ILUVW TXDQWLILFDWLRQ VWDQGDUG 4. ,QMHFW / IURP -10 samples (1-10 in a sample set). 5. ,QMHFW / IURP WKH VHFRQG TXDQWLILFDWLRQ VWDQGDUG 6. Compare the ratio (response factor) of the cyfluthrin / [ 2 H6]cyfluthrin peak area of each sample extract solution to the average ratio of the respective peak area of the quantitation standards on either side. 7. Compare the ratio of the cyfluthrin / [ 2 H6]cyfluthrin peak area of the quantitation standard injected before and after each group of sample extract solution injections. If the ratios vary by > 20% of the ratio of the first quantitation standard, prepare new aliquots of the quantitation standard and sample extract solutions and repeat steps 1 through 6. If there is < 20% variation, proceed to part C. C. Calculations 1. Compare the GC retention time of cyfluthrin / [ 2 H6]cyfluthrin in each of the injections made. The retention time of the cyfluthrin should be within ± 0.03 min of the [ 2 H6]cyfluthrin. Also, the retention time of the cyfluthrin in the sample injections should be with 0.10 min of the average of the retention times for the cyfluthrin in the sample extract’s respective quantitation standard injections. If these criteria are met, then proceed to Step 2. If not, then samples should be reanalyzed. 2. Calculate the concentration of cyfluthrin in each sample by comparing the detector response factor (peak area of cyfluthrin/[ 2 H6]cyfluthrin for the sample to the average response factor for the quantitation standards injected before and after the sample. response factor sample target sample weight ppm = X X standard conc. X dilution factor Avg standard response factor actual sample weight 37
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