Hiroyuki FUJITA 1 *, Takanori MAKINO1, Kenji INABA 1, Kazuki YAMAMOTO 2
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1 PAP2348_No14 Hiroyuki FUJITA 1 *, Takanori MAKINO1, Kenji INABA 1, Kazuki YAMAMOTO 2 1: MIURA CO., LTD., 864-1, Hojotsuji, Matsuyama, Ehime, , JAPAN; 2: Ehime University, 3-5-7, Tarumi, Matsuyama, Ehime, , JAPAN; Contact person;
2 We suggest a new simultaneous analysis for PCDDs / PCDFs / PCBs & PBDEs in food samples. In this presentation, we report a validated simultaneous analysis combined of the system and GC-HRMS for the monitoring of PCDDs / PCDFs / PCBs & PBDEs in food oil. This report mainly shows applications of the PBDEs measurement method with use of the system. Based on the results of quality control (QC) samples, real samples (unknown), procedure blanks, and certified reference material (CRM) samples, this report is discussed RSD, LOQ, trueness and recovery of PBDEs in PCB fractions obtained from the system. The GO-HT system may perform simultaneous analysis of PBDEs together with dioxins and PCBs in food fat. Trueness obtained by use of CRM is within ±2%. 29-decaBDE s blank is very low. The minimum recovery is 54% of 29-decaBDE. However, 29-decaBDE s recoveries in some of unknown samples are below 4%. We guess one reason why the low recovery is caused by purification shortage on purification columns. There is a necessary to keep studying ruggedness and stability of this simultaneous analysis.
3 Sample ID Code from What for? Cod Liver Oil EDF-5462 CIL Inc., Trueness, Repeatability, Recovery QC sample Fish Oil (Menhaden) F82-1L PFAD Pork fat Egg fat 3L / 4-Br( C 12 )diphenyl ether 15L / 4,4 -DiBr( C 12 )diphenyl ether 28L / 2,4,4 -TriBr( C 12 )diphenyl ether Internal STD 47L / 2,2,4,4 -TetraBr( C 12 )diphenyl ether 99L / 2,2,4,4,5-PentaBr( C 12 )diphenyl ether Recovery STD Wellington Laboratories Inc., : BDE-CVS-G/MBDE-MXG-STK/MBDE-ISS-G-STK/BDE-MXE 1L / 2,2,4,4,6-PentaBr( C 12 )diphenyl ether 126L / 3,3,4,4,5-PentaBr( C 12 )diphenyl ether 153L / 2,2,4,4,5,5 -HexaBr( C 12 )diphenyl ether 154L / 2,2,4,4,5,6 -HexaBr( C 12 )diphenyl ether 183L / 2,2,3,4,4,5,6-HeptaBr( C 12 )diphenyl ether 197L / 2,2,3,3,4,4,6,6 -OctaBr( C 12 )diphenyl ether 27L / 2,2,3,3,4,4,5,6,6 -NonaBr( C 12 )diphenyl ether 29L / DecaBr( C 12 )diphenyl ether SIGMA an EU laboratory Freeze-dried & Soxhlet extracted (7:3/Tol:Ace) (in our laboratory) 2 ppb 4 ppb 1 ppb Added amount 4 μl in Decane Ruggedness(minor changes), Recovery 79L / 3,3,4,5 -Tetra-Br( C 12 )diphenyl ether 8L / 2,2,3,4,4,5 -Hexa-Br( C 12 )diphenyl ether 26L / 2,2,3,3,4,4,5,5,6-Nona-Br( C 12 )diphenyl ether 2 ppb 4 ppb 1 ppb
4 Gas Chromatography Agilent 689N GC Column GC temp. program Total Time Inlet Carrier Gas Non-polar fused silica capillary column 1.5m + DB-5HT (15m,.25mmID x.1μmfilmthickness) 5 C(3min) 1 C/min 215 C (min) 5 C/min 28 C (min) 2 C/min 325 C (3.75min) 3 min Injection Vol.:2μL, 26 C, Splitless He, Constant Flow1.2 ml/min Transfer Line Non-polar fused silica capillary column 1m, 28 C Mass Spectrometer JMS-8 (JEOL Co., Ltd.) Ionization EI, Chamber Temperature 28 C, Voltage38eV, Emission Current 5μA, Maximum Acceleration Voltage 1kV Gruop1: Gruop2: Gruop3: Gruop4: Gruop5: Gruop6: Start time [min] MoBDEs / C12-MoBDEs / DiBDEs / C12-DiBDEs / TrBDEs /47.86 C12-TrBDEs / TeBDEs / C12-TeBDEs / PeBDEs / C12-PeBDEs / HxBDEs / C12-HxBDEs / HpBDEs / C12-HpBDEs / OcBDEs / C12-OcBDEs / NoBDEs / C12-NoBDEs / DeBDE / C12-DeBDE / Lock Mass
5 Add.5 ml to 2mL of Ethyl Acetate (C 4 H 8 O 2 ) : used primarily as a solvent and diluents, being favored because of its low cost, low toxicity, and agreeable odor. Setting the column up to the system Because adsorption activity of the silica gel in the purification column is too strong for PBDEs, when applying sample, it is necessary to add a polar-solvent in the sample solutions, for example, Ethyl Acetate, Dichloromethane or Diethyl ether. Also, it is necessary to pay attention that additive amount of the polar solvents will vary depending on the sample volume as follows. Conditioning of column Fat Sample Ethyl Acetate 15 to 2 ml of Hexane 1 g 1 g to 2.5 g 2.5 g to 3.5 g 2 ml 1mL to 1.5 ml.5 ml to less than 1 ml
6 Standard 2ppb x 2μL injection Quantity detected in a low level sample 1Br 2.4xe6 #3-BrDE 3.1xe xe6 1xe4 2Br 1.6xe #7-diBrDE #15-diBrDE 4.8xe #15 : S/N=8 (.4 pg) xe6 1.6xe Br 1xe6 #17-triBrDE #28-triBrDE 3.5xe3 #28 : S/N=6.7 (.9 pg) xe5 8xe Br 5xe5 #49 #71 #47 #66 # xe4 #47 : S/N=7 (2.5 pg) xe5 4xe Br 3xe5 3xe5 #1 #99 #85 #126 # xe4 #99 : S/N=116 (3.4 pg) xe
7 Standard 2ppb x 2μL injection Quantity detected in a low level sample 6Br 6xe5 #154 #153 #8 8xe3 #153 : S/N=18 (1.3 pg) xe5 4xe Br 8xe4 #184 #183 # xe3 #183 : S/N=5 (1.7 pg) xe5 8xe Br 1.2xe5 #197-octaBrDE #196-octaBrDE xe3 8 #196 : S/N=5 (2.2 pg) xe5 8xe4 9Br 2.5xe5 2xe #27-octaBrDE #26-octaBrDE xe #26 : S/N=7.5 (5.6 pg) xe Br 5xe4 #29-decaBrDE #29 : S/N=2 (37 pg) xe4 2xe
8 pg/g fat Sample CIL EDF-5463 Cod liver oil 1 g Blank Egg fat Reference Value Results by using GO-HT AcEt 1mL AcEt 2mL Estimated LOQ isomers Assigned ± SD x 2 N=1 N=2 N=3 N=4 Average SD RSDr Deviation N=1 N=2 by S/N3 [pg] #3-MoBDE #15-DiBDE % - ND ND #17-TriBDE 8.83 ± % -19% ND ND.2 to.1 #28-TriBDE 4.1 ± % -5% ND ND #47-TeBDE 148 ± % 1% ND ND #66-TeBDE 48.4 ± % 3% ND ND #1-PeBDE 357 ± % -2% ND ND.1 #99-PeBDE 193 ± % -17% ND ND #154-HxBDE 229 ± % -1% ND ND #153-HxBDE 33.9 ± % -5% ND ND #183-HpBDE % - ND ND #197-OcBDE - - ND ND ND ND ND ND 1-2 #196-OcBDE - - ND ND ND ND ND ND #27-NoBDE % - ND ND #26-NoBDE % - ND ND #29-DeBDE % - ND ND 5 to 1 Recovery #3-MoBDE #15-DiBDE #28-TriBDE #47-TeBDE #99-PeBDE #154-HxBDE #153-HxBDE #183-HpBDE #197-OcBDE #27-NoBDE #29-DeBDE
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