Shimadzu Techno-Research Inc., Japan - UNEP Chemicals

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Cleanup of POPs Basically applied Florisil clean up �� H2SO SO4 or 22%-H 22% 2SO SO4/Silica /Silica��degradation degradation of Dieldrin and Endrin �� 44%- 44% H2SO SO4/Silica /Silica�� degradation of Aldrin and Heptachlor epoxide. Useful cleanup for Stable POPs(DDT & HCH etc) �� AgNO 3/Slica /Slica�� degradation of Heptachlor, low recovery of MoCB �� DMSO/Hex. partitioning��a partitioning a little low recovery of HCB and Aldrin �� Volatile POPs��HCB POPs HCB��HCHs HCHs��Heptachlor Heptachlor��Aldrin Aldrin�� MoCB Biological sample cleanup SHIMADZU TECHNO RESEARCH, Inc. � Stable POPs compounds�H2SO4/slica is effective after Florisil cleanup, only stable POPs for acid � Florisil cleanup� less polar fraction 20%-DCM/Hex. & polar fraction (Heptachlor epoxide, Dieldrin, Endrin) DCM fr. (much better clean up compare to ether fr.) � High lipid content sample �insufficient cleanup cause to broad GC peak � DMSO/Hex. partitioning�effective for lipid & mineral oil & aliphatic hydrocarbons � LOD 0.05�0.2ng/g SHIMADZU TECHNO RESEARCH, Inc.
�� DMSO/Hex. partioning��effective partioning effective for air & sediment mineral oil & aliphatic hydrocarbons �� Ultra high level congeners��major congeners major PCB, p,p‘-DDE, p,p DDE, p,p’-DDD p,p DDD saturated peak, memory effects in the GC column, separate analysis for different analyte with cleanup factor �� Blank of POPs�� POPs HCB��Chlordane HCB Chlordane & BFR(HBB, DeBDE), endsulfan, great care should be taken for the laboratory dust �� HCB & chlordane has relatively high method blank level��pg level pg��on on the other hand low level in the biological sample SHIMADZU TECHNO RESEARCH, Inc. Experiences of sample for POPs analysis by HRGC/HRMS Insufficient cleanup �� Broad GC peak shape : dirty Ion source & liner �� Variation of ionization efficiency, sensitivity, change of ion intensity of fragment ions, variation of monitor ions, degradation & adsorption in the GC column �� cleanup is most important for HRMS analysis Unstable POPs affect variation of sensitivity : Endrin, Endrin, Heptachlor, DDT �� Strongly recommended use of 13 13C C internal standards, standards but variation of sensitivity and recovery % should occur even though stable RRF �� interference of PBDE(Tetra) to PCB(Penta) on HT-8 HT GC column SHIMADZU TECHNO RESEARCH, Inc.
Page 1 and 2: Waters TOF Meeting at Dioxin2008, T
Page 3 and 4: Summary of our capability �� 11
Page 5 and 6: New New POPs POPs proposed POPs �
Page 7 and 8: Control by Database system �� A
Page 9 and 10: median, NIQR, CV% rob, min., max.,
Page 11 and 12: pg-TEQ 900 850 800 750 700 650 600
Page 13 and 14: Typical Interferences in Dioxin ana
Page 15 and 16: 100% 90% 80% 70% 60% 50% 40% 30% 20
Page 17 and 18: PCB fragment ion and PCDD ion P(n)
Page 19 and 20: Usage in Japan (ton) 1946-1972 1,00
Page 21 and 22: POPs concentrations in air sample
Page 23 and 24: HRGC/HRMS Micromass Autospec Ultima
Page 25 and 26: Native Standard Internal Standard o
Page 27 and 28: 1.20 1.10 1.00 0.90 0.80 0.70 0.60
Page 29 and 30: pg 100 10 1 0.1 0.01 0.02 0.02 TCDD
Page 31 and 32: Internal standard : different bromi
Page 33 and 34: 051019XO1001 19-Oct-2005 14:39:45 V
Page 35: MDL & MDL of air sample by HRMS sam
Page 39: pg/g lipid Major POPs in Human Bloo

Shimadzu Techno-Research Inc., Japan - UNEP Chemicals

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