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

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Bayer Corporation <strong>108139</strong>-1 Agriculture Division 3.3.3 Linearity Standard Solutions Linearity standards consist of a mixture of the cyfluthrin and [ 2 H6]cyfluthrin. The [ 2 H6]cyfluthrin concentration was held constant in each linearity standard (same level used in the sample analysis) while the cyfluthrin concentration was varied from the lowest designated point to the highest designated point. 3.3.3.1 Linearity Standards 0 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.002 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.004 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR a 50-mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.010 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.020 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.050 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.10 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 0.20 ppm Add 1.0 mL of the 2.5 J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 1.0 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG and 10.0 mL of the J P/ VHFRQGDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 30
Bayer Corporation <strong>108139</strong>-1 Agriculture Division 5.0 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ VHFRQGary standard to a 50-mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 10.0 ppm $GG P/ RI WKH J P/ GHXWHUDWHG VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ SULPDU\ VWDQGDUG WR D -mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 3.3.4 Quantification Standard 4XDQWLILFDWLRQ 6WDQGDUG J P/ $GG P/ RI WKH J P/ VHFRQGDU\ VWDQGDUG DQG P/ RI WKH J P/ deuterated secondary standard solution to a 50-mL volumetric flask. Dilute the solution to volume with toluene. Mix the solution thoroughly. 3.4 Analytical Method 3.4.1 Matrix Preparation 1. Add approximately 2.5 lbs of the raw agricultural commodity (RAC) to the vertical batch processor. Add about an equal portion of palletized dry ice to the sample in the processor. Macerate the combined dry ice and RAC until a homogenous mixture is obtained. 2. Pour the homogenized mixture into a plastic Tupperware container and store open at –20 ± 5 °C until the last traces of dry ice have sublimed. Store the homogenized RAC in a freezer at –20 ± 5 °C. 3.4.2 Procedure (Apples and Pears only) 3.4.2.1 Extraction 1. Weigh 5.0 g of sample into a 120-mL glass bottle. Note: begin recovery samples at this point by fortifying the control matrix sample with a standard. 2. Add 45 mL of the solvent mixture MeOH/aqueous 1.2 N HCl (4:1, v/v) into the bottle. Homogenize for 2 min using a tissumizer. 3. Vacuum filter the sample solution using a Buchner funnel into a stoppered 100-mL graduated cylinder. 4. Return the solids including the paper filter back to the glass bottle, and add 31
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