LAAN-A-LM-E050 Liquid Chromatography Mass Spectrometry No.C79 Analysis of Polymer Additives Using the LCMS-8030 Triple Quadrupole LC/MS/MS Antioxidants, ultraviolet absorbers, flame retardants and other polymer additives are indispensable for improving the characteristics and functionality of polymers. Understanding the types and quantities of these additives to be used is extremely important to effectively control the manufacturing process of the polymers. Below is an example of quantitative analysis of 14 types of polymer additives using MRM (Multiple Reaction Monitoring) and the LCMS-8030 triple quadrupole mass spectrometer. n MRM Analysis with the LCMS-8030 Conducting MRM measurement with a triple quadrupole mass spectrometer makes it possible to obtain molecular structure information while simultaneously performing quantitative analysis. Fig. 1 shows the chromatograms of 14 polymer additives. Two additives were analyzed in positive mode, and 12 were analyzed in negative mode. Fig. 2 shows the calibration curves of each of the constituents. Excellent linearity was obtained for every compound tested. (×10,000,000) 1.25 Irganox 245 585.30>367.20(-) Irganox 1098 635.45>417.50(-) Irganox MD 1024 1.00 Tinuvin P 226.10>107.10(+) Cyanox 2246 0.75 339.15>163.20(-) Cyanox425 367.25>177.20(-) Irganox 1035 Irgafos 168 oxide 0.50 Tinuvin 120 Irganox 1010 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 663.50>57.15(+) 437.25>205.25(-) 350.25>319.85(-) Irganox 1330 773.55>773.55(-) Irganox 1076 529.45>41.15(-) Irganox 565 0.00 641.35>83.20(-) 1175.70>1175.70(-) Tinuvin 328 0.25 551.35>333.40(-) 587.35>58.10(-) 7.0 min Fig. 1 Chromatograms of 14 Polymer Additives Irganox 245 3.0 Irganox MD 1024 面積(×100,000) 1-500 ppb 2.5 2.25 1.00 R^2=0.995 0 100 200 300 400 濃度 0.00 Cyanox 425 500 750 濃度 7.0 5.0 R^2=0.996 0 100 200 300 400 5-500 ppb 2.0 0.5 R^2=0.997 0.0 25.0 50.0 75.0 濃度 0.0 0.0 Tinuvin 328 25.0 50.0 75.0 濃度 500-10000 ppb 1.0 0 2500 5000 7500 濃度 300 400 濃度 6.0 0 2500 5000 R^2=0.998 7500 濃度 0.00 0.0 25.0 50.0 75.0 濃度 Irganox 1076 1-1000 ppb 3.0 1.5 1.0 100 200 300 400 濃度 0.5 0.0 75.0 濃度 0.1-100 ppb 2.0 R^2=0.997 2.5 0 50.0 3.0 3.5 R^2=0.996 25.0 4.0 0.25 0.00 0.0 5.0 面積(×100,000) 0.5-500 ppb 0.25 0.5 0.0 200 0.50 1.5 R^2=0.999 0.01-100 ppb 2.0 2.0 0.50 100 0.75 2.5 0.75 0 0.0 Irganox 1010 0.50 R^2=0.996 R^2=0.997 0.5 面積(×10,000) 0.75 1.00 3.0 濃度 1.00 面積(×1,000,000) 0.5-10000 ppb 3.5 750 Tinuvin 120 Irganox 565 面積(×1,000,000) 4.0 1.00 0.25 0.0 500 1.25 1.0 Irganox 1330 面積(×100,000) 1.25 R^2=0.998 1.0 250 面積(×1,000,000) 1.50 2.0 3.0 1.0 R^2=0.999 1.75 3.0 4.0 1.5 0 面積(×10,000) 4.0 5.0 1.0 2.0 0.5 濃度 6.0 1.5 2.5 1.0 Irgafos 168 oxide 0.5-100 ppb 8.0 2.0 0.00 250 面積(×10,000) 0.01-100 ppb 2.5 0 0.00 0.01-100 ppb 3.0 1.5 0.25 Irganox 1035 面積(×1,000,000) 3.0 R^2=0.997 0.25 3.5 2.0 0.50 0.50 Cyanox 2246 面積(×1,000,000) 1-1000 ppb 2.5 0.75 0.5 0.0 5-500 ppb 0.75 1.25 1.0 Tinuvin P 面積(×100,000) 面積(×100,000) 1.00 1.50 1.5 0.0 1-1000 ppb 1.75 2.0 Irganox 1098 面積(×100,000) 2.00 R^2=0.999 0 250 500 Fig. 2 Calibration Curves of 14 Polymer Additives 750 濃度 1.0 0.0 R^2=0.997 0.0 25.0 50.0 75.0 濃度 No.C79 n Analysis of Unknown Polymer Additives Using the LCMS-8030 Quantitative analysis was conducted for the polymer additives in a food wrapping material and food container. THF (1 mL) was added to a pulverized sample (0.1 g), and this was sonicated for 1 minute. The supernatant was collected, 1 mL of 5 mM ammonium acetate was added, and the final mixture was filtered (0.45 μm.) Fig. 3 shows the MS chromatograms and the MRM Food Wrapping Material (×10,000) Food Container (×100,000) 4.0 7.0 3.5 6.0 3.0 5.0 2.5 4.0 2.0 3.0 1.5 2.0 1.0 1.0 0.5 0.0 0.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 min 2.5 (×1,000) 4.859 2.0 1.5 4.0 4.5 49.7 ng/g 0.5 0.5 4.7 4.8 4.9 0.6 14.3 μg/g 6.5 7.0 min (×1,000) 48.7 ng/g 0.4 0.2 3.1 3.2 3.3 3.4 Irganox 245 Fig. 3 Chromatograms of Polymer Additives Detected in the Analysis (Left) Food Wrapping Material, (Right) Food Container Table 1 Analytical Conditions : Shim-pack XR-ODS Ⅱ (75 mmL. × 2.0 mmI.D., 2.2 μm) : 0.1 % formic acid : Methanol : 25 %B (0 min) - 100 %B (2.5-7.5 min) - 25 %B (7.51-10 min) : 0.5 mL/min : 2 μL : 40 °C : SHIMADZU LCMS-8030 : +4.5 kV (ESI-Positive mode), –3.5 kV (ESI-Negative mode) Nebulizing Gas Flow : 1.5 L/min Drying Gas Pressure : 10 L/min : 250 °C DL Temperature : 400 °C BH Temperature For Research Use Only. Not for Use in Diagnostic Procedures. SHIMADZU CORPORATION. International Marketing Division 6.0 0.8 Irganox 1010 Column Mobile Phase A Mobile Phase B Gradient Program Flow Rate Injection Volume Column Temperature MS Probe Voltage 5.5 1.0 0.0 5.0 5.0 1.2 1.0 1.5 0.0 3.5 (×100,000) 2.5 1.0 3.0 4.863 3.0 3.258 2.5 chromatograms of the substances detected. The concentrations of each of the constituents calculated using the calibration curves of Fig. 2 were determined to be 49.4 ng/g of Irganox 1010 detected in the food wrapping material, and 14.3 μg/g of the Irganox 245 and 48.7 ng/g of Irganox 1010 detected in the food container. 3. Kanda-Nishikicho 1-chome, Chiyoda-ku, Tokyo 101-8448, Japan Phone: 81(3)3219-5641 Fax. 81(3)3219-5710 4.7 4.8 4.9 Irganox 1010 5.0
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