IN THE UNITED STATES PATENT AND TRADEMARK OFFICE
`
`
`In re Inter Partes Reexamination of U.S. Patent No. 8,030,348
`
`
`Entitled:
`
`NATURAL MARINE SOURCE PHOSPHOLIPIDS COMPRISING
`POLYUNSATURATED FATTY ACIDS AND THEIR APPLICATIONS
`
`4 October 2011 to Sampalis
`
`
`Issued:
`
`Control No.: 95/001,774
`
`Filed:
`
`Examiner:
`
`October 19, 2011
`
`Bruce Campbell
`
`
`
`FIRST SUPPLEMENTAL DECLARATION BY DR. THOMAS
`GUNDERSEN IN SUPPORT OF REQUEST FOR INTER PARTES
`REEXAMINATION OF U.S. PATENT NO. 8,030,348
`
`
`EFS WEB Filed
`
`Mail Stop Inter Partes Reexam
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
`
`
`I, Dr. Thomas Gundersen, state as follows:
`
`1. My present position is CEO of Vitas AS - Analytical Pharma Services, Oslo, Norway.
`
`My Curriculum Vitae is attached hereto as Exhibit 1.
`
`2.
`
`In 2011, I was asked by Aker Biomarine ASA to analyze lipid fractions extracted from
`
`two species of krill, Euphausia superba and Euphausia pacifica, to determine whether they
`
`contain phospholipids that have either eicosapentaenoic acid (EPA) or docosahexaenoic acid
`
`(DHA) at both the sn-1 and sn-2 positions of the phospholipid molecule. I performed this
`
`analysis which was the subjection of my Declaration dated October 4, 2011. Exhibit 2 to my
`
`2011 Declaration was a laboratory report on the analysis. This report contained two sets of data
`
`presented in Appendix A and Appendix B. The data in Appendix A of my 2011 report is HPLC-
`
`
`
`1
`
`000001
`
`

`
`MS data which was used for preliminary analysis of the samples to determine if they contained
`
`phospholipid species with the appropriate molecular weights. The data in Appendix B of my
`
`2011 report is HPLC-MS/MS (MRM) which definitively identifies the individual phospholipid
`
`species contained in the samples that were analyzed. The Appendix A data contained unintended
`
`mistakes (due to a cut and paste error when putting the report together) in the last panels
`
`presented for samples P308-8, P308-9, P308-10, P308-11, and P308-12. These mistakes do not
`
`affect the conclusions I reached with respect to the presence of the phospholipid species in the
`
`samples, which were based on the data presented in Appendix B of my 2011 report. Exhibit 2
`
`attached hereto contains the corrected Appendix A data and original Appendix B data. The
`
`corrected Appendix A data is entirely consistent with the conclusions presented in my 2011
`
`Declaration and Report, the results of which are summarized in the Table below which was
`
`provided with my 2011 Declaration.
`
`MRMs
`
`Vitas
`
`Frac.
`
`Treatment
`
`[825+H]→184
`
`ID
`
`#
`
`°C/min
`
`[851+H]→184
`
`MRM
`
`MRM
`
`MRM
`
`MRM
`
`1
`
`PC-
`
`2
`
`PC-
`
`3
`
`PC-
`
`4
`
`PC-
`
`[877+H]→184
`
`EPA/EPA
`
`EPA/DHA
`
`EPA/DHA
`
`DHA/DHA
`
`826→524
`
`852→524
`
`852→550
`
`878→550
`
`Conclusion
`
`P308-1
`
`
`
`
`
`IIa
`
`none
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-EPA/EPA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`P308-2 IIa
`
`70/5
`
`P308-3 IIa
`
`125/15
`
`P308-4
`
`
`
`
`
`IIb
`
`none
`
`P308-5 IIb
`
`70/5
`
`P308-6 IIb
`
`125/15
`
`
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`NO
`
`NO
`
`NO
`
`NO
`
`NO
`
`NO
`
`NO
`
`NO
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`n.d. PC-EPA/EPA
`
`NO
`
`NO
`
`NO
`
`NO
`
`n.d. PC-EPA/DHA
`
`n.d. PC-DHA/DHA
`
`n.d. PC-EPA/EPA
`
`NO
`
`NO
`
`NO
`
`NO
`
`n.d. PC-EPA/DHA
`
`NO
`
`NO
`
`NO
`
`NO
`
`n.d. PC-DHA/DHA
`
`n.d. PC-EPA/EPA
`
`n.d. PC-EPA/DHA
`
`2
`
`000002
`
`

`
`P308-7
`
`
`
`
`
`IIa
`
`none
`
`P208-8 IIa
`
`70/5
`
`P308-9 IIa
`
`125/15
`
`P308-
`
`
`
`
`
`10
`
`IIb
`
`none
`
`P308-
`
`11
`
`IIb
`
`70/5
`
`NO
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`n.d. PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`P308-
`
`12
`
`P308-
`
`13
`
`P308-
`
`14
`
`P308-
`
`15
`
`P308-
`
`16
`
`IIb
`
`125/15
`
`n.a.
`
`n.a.
`
`n.a.
`
`n.a.
`
`n.a.
`
`n.a.
`
`n.a.
`
`n.a.
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`Contains PC-EPA/EPA
`
`YES
`
`YES
`
`YES
`
`YES
`
`Contains PC-EPA/DHA
`
`Contains PC-DHA/DHA
`
`3
`
`
`
`
`
`000003
`
`

`
`3.
`
`The results presented in my 2011 Declaration do not suffer from a carry-over effect. I
`
`did include standard blanks in my analysis, but did not include that data in the original report as
`
`it was of minor importance and as it is not customary. Exhibit 3 attached hereto provides two
`
`examples demonstrating the absence of carry-over effect. In the first example, the highest
`
`standard is analyzed before a solvent blank. In the other example, a solvent blank is analyzed
`
`directly after a sample. The time and date of the analysis on the original data proves that these
`
`are run in series and that these controls were run in the very same sequence as the original
`
`samples. As can be seen, there are no carry over or memory effects. Carry-over effects are not
`
`expected as the design of the injector is of the ”flow through principle” meaning that the mobile
`
`phase is flowing through the autosampler needle for most of the analysis time of 18 minutes ( in
`
`this case). The needle is also flushed on the outside in a “wash station” before the next injection.
`
`The HPLC used in the LC-MS (SQ) method is the type same as for the LC-MS/MS method.
`
`Carry-over was not an issue in these experiments.
`
`4.
`
`Dr. Jaczynski argues that the setup used by Gundersen works through air-liquid
`
`convection and that this renders it unsure if the oil really was heated to 125 degrees Celsius for
`
`15 minutes or 75 degrees for five minutes. This assumption is probably drawn because Dr.
`
`Jaczynski hasn’t understood the experimental setup in detail and thereby what heat transfer
`
`principle is actually applied. The heating of the lipid was performed in a 12 mm outer diameter
`
`1.8 ml flat bottom glass vial. The metal heat block has flat bottom holes that match the vials
`
`perfectly with regards to outer diameter and depth. Thus, there is close contact with the bottom
`
`of the vial and the bottom of the heat block hole as well as the walls of the vial and the walls of
`
`the heat block hole. The oil in the vial is a small amount covering the bottom of the vial. The
`
`heat transfer is from the preheated metal heat block through the thin glass wall of the vial,
`
`primarily the bottom, and directly into the oil. It is thus not an air-liquid convection as stated by
`
`Dr. Jaczynski. Covering the vials with aluminum foil is not necessary as the setup is inside the
`
`oven with 125 degrees ambient temperature. The temperature of the small amount of oil reaches
`
`125 degrees in seconds using this principle. Using the analogy of Dr. Jaczynski, this type of
`
`heating would be similar to touching the metal sides inside the kitchen oven and that this off
`
`course will cause rapid severe pain indicating very efficient heat transfer.
`
`
`
`4
`
`000004
`
`

`
`5.
`
`I further declare that all statement made herein of my own knowledge are true and that all
`
`statements made on information and belief are believed to be true; and further that these
`
`statements were made with the knowledge that willful false statements and the like so made are
`
`punishable by fine or imprisonment, or both, under section 1001 of title 18 of the United States
`
`Code, and that such willful false statements may jeopardize the validity of the application or any
`
`patent issued thereon.
`
`
`
`Respectfully submitted,
`
` Dr. Thomas Gundersen
`
`
`
`
`
`
`
`Date: April 18, 2012
`
`
`
`5
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`
`000005
`
`

`
`       
`
`EXHIBIT 1 
`
`EXHIBIT 1
`
`000006
`
`000006
`
`

`
`CURRICULUM VITAE OF THOMAS E GUNDERSEN
`
`
`
`
`
`
`
`
`
` Personal
`
` Name: Thomas Erik Gundersen
`
` Born: August 4th 1967
`
` Address: Lillevannsveien 69B, 0788 Oslo
`
` Phone: +47 22 95 86 31/ +47 928 08 973
`
`E-mail: teg@vitas.no
`
` Marital status: Married, 3 children
`
` Education
`
`1990-1995: M.Sc. in Chemistry, majoring in Analytical Chemistry,
`University of Oslo. Title of thesis: Quantitative high performance liquid
`chromatographic determination of retinoids in human serum using on-line solid
`phase extraction and column switching. Rating 1.2 (on a scale from 1-6 where
`1 is best)
`
` 2007 Dr. Philos ( PhD) at the Medical Faculty, University of Oslo. 8
`published articles. Title: "Development of ultra-sensitive chromatographic
`tools for high-throughput analysis of retinoids in biological samples"
`
`Trial lecture: Lipidomics - Recent technological developments and
`applications
`
` Relevant work experience
`
` 01/01/1998 to 12/31/2001: Recruitment Fellow of the Norwegian Cancer Society at the
`Institute for Nutrition Research, University of Oslo.
`
` 2002 to 2004 Research Fellow at the Institute for Nutrition Research, University of Oslo.
`
`2005-2008 Researcher at the Institute for Nutrition Research, University of Oslo.
`
` 2002 - General manager of Vitas' s
`
` 2007 - General Manager Bioindex as
`
`2008 – 2011 Senior Researcher at the Medical Faculty, University of Oslo ( 20/40 %)
`
`
`
`000007
`
`

`
` Courses:
`
` Gas Chromatography, 1997 1 day
`
` HPLC-Chemstation, 1998 1 day
`
`Capillary electrophoresis, 1998 2 days
`
` LC-MS, 1999 1 day
`
` LC-MS, 2000, one day
`
`LC-MS/MS, 2005 3 days
`
` HSE Course for Directors, 2008 1 day
`
` GMP, one day in 2008
`
` Teaching and tutoring
`
`Supervisor for graduate students Sakhi Amrit K, Stein Joakim Thommesen and Erasmus
`exchange student Carsten Haas in the period 1998-2001.
`
` Supervisor for doctoral students Amrit K Sakhi and Olov Nordstrom in the period 2001-2003.
`
` Supervisor for doctoral students Bente Lise Halvorsen and Anette Karlsen in the period
`2002-2008.
`
` The head of the analytical "subgroup" consisting of a total of 5 persons in Rune Blomhoff's
`research group at the Institute for Nutrition Research, University of Oslo. In the period 2000-
`2006
`
` Assistant supervisor for Post-Doc Sakhi Amrit K. and E. Nasser Bastani Fellow during 2008.
`
`Invited work
`
` a) Review, Gundersen, TE & Blomhoff, R., On-line solid-phase extraction and isocratic
`separation of retinoic acid isomers in micro drilling column switching system. Methods
`Enzymol 299:430-41, 430-441 (1999).
`
` b) Review, Gundersen, TE & Blomhoff, R., Qualitative and Quantitative liquid
`chromatographic determination of natural retinoids in biological samples. J Chromatogr A.
`2001 November 1923, 935 (1-2) :13-43.
`
` c) Review, Gundersen, TE, Methods for Detecting and Identifying retinoids in tissue. J
`Neurobiol. 2006 June; 66 (7) :631-44.
`
`
`
`000008
`
`

`
` Other activities
`
`Founded in 1994 AS Vitas, together with Professor Rune Blomhoff and Professor Christian A
`Drevon. AS Vitas is GMP certified analytical CRO that offers services to Academia,
`Pharmaceutical and biotech industry, hospitals and the Norwegian primary health care. The
`company is located in Oslo Innovation Centre. The analysis methods used are a direct result
`of graduate and doctoral work of Thomas Gunderson.
`
` Thomas Gundersen have from 1994 until today been central in the daily operation and
`development of business strategy and analysis in AS Vitas, and is part owner of the company.
`CEO of AS Vitas, 1 February 2002 -
`
` Founded in December 2006 the company Bioindex AS together with the technology transfer
`office of UIO. Thomas Gunderson sat on the board of Bioindex AS start-up to September
`2007. CEO of Bioindex AS.
`
` "Expert reviewer” of fat-soluble vitamins in Finland Labquality external quality assurance
`program from September 2009 -
`
` Principal Scientist in EU projects:
`
` 1. Food4Me - 2011-2015 - Coordinated by University College Dublin, Ireland.
`
` 2. EPIC-CVD - 2012-2016 - Coordinated by University of Cambridge, UK.
`
` 3. Nutri Tech - 2012-2016 – Coordinated by TNO, Holland.
`
`
`
`
`
`Publications
`
` 1 Gundersen, T. E., Lundanes, E. & Blomhoff, R. J Chromatogr B.Biomed.Sci.Appl. 691,
`1943-1958 (1997).
`
` 2. Holven, KB, Natarajan, V., Gundersen, TE., Moskaug, JO, Norum, KR & Blomhoff, R.
`Int. J Cancer 71, 654-659 (1997).
`
` 3. Sakhi, AK, Gundersen, TE., Wolf, SM, Blomhoff, R. & Lundanes, E.. J Chromatogr. A
`828, 451-460 (1998).
`
` 4. Christensen, EI, Moskaug, JO, Vorum, H., Jacobsen, C., Gundersen, TE., Nykjaer, A.,
`Blomhoff, R., J Am Soc Nephrol 10, 685-695 (1999).
`
` 5 Gunderson, T. E. & Blomhoff, R. Methods Enzymol 299:430-41, 430-441 (1999).
`
` 6. P. Molander, TE Gundersen, C. Haas, T. Greibrokk, R. Blomhoff, E. Lundanes, Journal
`of Chromatography A 847, No. 1-2, 25 1999 59-68
`
`000009
`
`

`
` 7. P. Molander, SJ Thommesen, IA Bruheim, R. Trones, T. Greibrokk, E. Lundanes, TE
`Gundersen, HRC Journal of High Resolution Chromatography, 22, Nr. 9, September 1999,
`pages 490-494
`
` 8. Ulven SM, Gundersen TE, Weedon MS, Landaas VO, Sakhi AK, Fromm SH, Geronimo
`BA, Moskaug JO, Blomhoff R, Dev Biol 2000 in April 1915, 220 (2) :379-91
`
` 9. SM. Ulven, TE. Gundersen, AK. Sakhi, JC. Glover and R. Blomhoff, Dev Dyn. 2001
`November; 222 (3) :341-53.
`
` 10. F. Hoover, TE Gundersen, SM Ulven, J. Micha Ille, S. Blanchet, R. Blomhoff and JC
`Glover, J Comp Neurol. 2001 in July 1930, 436 (3) :324-35
`
` 11 TE Gundersen and R. Blomhoff, J. Chromatogr A. 2001 November 1923, 935 (1-2) :13-
`43
`
` 12. Petrosian AM, Haroutounian JE, Gundersen TE, Blomhoff R, Fugelli K, Kanli H.
` Adv Exp With Biol. 2000; 483:453-60.
`
` 13. Capillary High-Performance Liquid Chromatographic determination of lutein and
`zeaxanthin in aqueous humor from a single mouse eye. Anette Karlsen, George Alexander;
`Rune Blomhoff and Thomas E Gundersen. 1: J Chromatogr B analyte Technol BioMed
`Life Sci. 2003 in September 1925, 795 (1) :17-23.
`
` 14. Identification of novel roles of the cytochrome P450 system in early embryo genesis,
`effects Wed vasculogenesis and retinoic acid homeostasis. Diana ME Otto, Colin J.
`Henderson, Diane Carrie, Megan Davey, Ralf H. Adams, Cheryl Tickle, Thomas E.
`Gundersen, Rune Blomhoff and Rolan Wolf. Mol Cell Biol. 2003 September; 23
`(17) :6103-16.
`
` 15. Sakhi AK, Russnes KM, Smeland S, Blomhoff R, Gundersen TE., Simultaneous
`quantification of Reduced and oxidized glutathione in plasma needs something a two-
`dimensional chromatographic system with parallel Porous graphitized carbon columns
`coupled with fluorescence and coulometric electrochemical detection. J Chromatogr A. 2006
`February 3, 1104 (1-2) :179-89.
`
` 16. Karlsen A, Blomhoff R, Gundersen TE. High-throughput analysis of vitamin C in
`human plasma with the use of HPLC with monolithic column and UV detection. J
`Chromatogr B analyte Technol BioMed Life Sci. 2005 in September 1925, 824 (1-2) :132-8.
`
` 17. Drevon CA, Henriksen HB, Sanderud M, Gundersen TE, Blomhoff R. Biological
`effects of vitamin K and concentration of vitamin K in Norwegian food. Tidsskr Nor
`Laegeforen. 2004 Jun 17; 124 (12) :1650-4. Review.
`
` 18. Gundersen, TE., Methods for Detecting and Identifying retinoids in tissue. J Neurobiol.
`2006 June; 66 (7) :631-44.
`
`
`
`0000010
`
`

`
`
`
` 19. Sakhi AK, Blomhoff R, Gundersen TE. Simultaneous and trace determination of the
`Reduced and oxidized glutathione in minute plasma samples needs something dual mode
`fluorescence detection and column switching high performance liquid chromatography. J
`Chromatogr A. 2007 February 1923; 1142 (2) :178-84
`
` 20. Karlsen A, Blomhoff R, Gundersen TE.
` Stability of whole blood and plasma Ascorbic acid. Eur J Clin Nutr. 2007 Feb 7
`
` 21. TE Gundersen, NE Bastani, R. Blomhoff: Quantitative high-throughput determination
`of endogenous retinoids in human plasma needs something triple-stage liquid chromatography
`/ tandem mass spectrometry.Rapid commun Mass Spectrom. 2007; 21 (7) :1176-86.
`
` 22. Berhe N, Halvorsen BL, Gundersen TE, Myrvang B, Gundersen SG, Blomhoff R.
`Reduced serum concentration of retinol and alpha-Tocopherol and high concentration of
`hydroperoxides are Associated with community levels of S. mansoni infection and
`schistosomal periportal fibrosis in Ethiopian school children. Am J Trop With Hyg. 2007
`May; 76 (5) :943-9.
`
` 23. Noble BR, Babiuk RP, Clugston R, Underhill TM, Sun H, Kawaguchi R, Walfish PG,
`Blomhoff R, Gundersen TE, Greer JJ. Mechanisms of action of the congenital diaphragmatic
`hernia-inducing teratogen nitrofen. Am J Physiol Lung Cell Mol Physiol. 2007 August 1917
`
` 24. Katy Schmidt, Catherine Hughes, JA Chudek, Simon Goodyear, Richard Aspden,
`Richard Talbot, Thomas E. Gundersen, Rune Blomhoff, Colin Henderson, C. Roland Wolf
`and Cheryll Tickle. Cholesterol metabolism: the main pathway acting downstream of
`cytochrome P450 oxidoreductase in skeletal development of the limb. Molecular and cellular
`Biology, March 9 2009.
`
` 24. Kristoffer Ström and Thomas E. Gundersen, Ola Hansson, Stéphanie Lucas, Céline
`Fernandez, Rune Blomhoff, and Cecilia Holm. Hormone-sensitive lipase (HSL) is Also a
`Retinyl ester hydrolase: evidence from mice lacking HSL. FASEB J. February 2009.
`
` 25. Nasser Bastani, Thomas E. Gundersen and Rune Blomhoff. Determination of 8-epi
`PGF2α in human plasma, full blood, erythrocyte and urine needs something isotope dilution
`and triple-stage liquid chromatography / tandem mass spectrometry. Rapid commun Mass
`Spectrom. 2009 in August 1910, 23 (18) :2885-2890.
`
` 26. Trygve Holmøy 1.2, Stine Marit Moen 1, Thomas E. Gundersen 3, A Michael Holick
`January 4 Falch 5 Enrico Fainardi 6, Massimiliano 6, Ilaria Casetta 6. Vitamin D in
`cerebrospinal fluid from Patients with multiple sclerosis relapse and remission hum.
`Accepted by Multiple Sclerosis, February 2009, Published online September 2009.
`
` 27. Jaensson-Gyllenbäck E, Kotarsky K, Zapata F, Persson EK, Gundersen TE, Blomhoff
`R, Agace WW. Bile retinoids imprint intestinal CD103 (+) dendritic cells with the ability two
`gene ratio gut-tropic T cells. Mucosal Immunol. Mucosal Immunol. 2011 Jul;4(4):438-47
`
`28. Holmøy T, Lossius A, Gundersen TE, Moen SM, Castellazzi M, Fainardi E, Casetta I.
`Intrathecal levels of vitamin D and IgG in multiple sclerosis. Acta Neurol Scand. 2011 Jul 23
`
`0000011
`
`

`
`29. Bastani NE, Gundersen TE, Blomhoff R. Dried blood spot (DBS) sample collection for
`determination of the oxidative stress biomarker 8-epi-PGF(2α) in humans using liquid
`chromatography/tandem mass spectrometry. Rapid Commun Mass Spectrom. 2012 Mar
`30;26(6):645-52.
`
` Posters and oral presentations
`
` 1 Gundersen, T and Blomhoff, R., Automated chromatographic determination of fat-soluble
`vitamins. Oral presentation, 13th Norwegian symposium in chromatography, 1996.
`
` 2. Sakhi, AK, Gundersen TE, Ulven, SM, Blomhoff, R. & Lundanes, E Electrochemical
`detection of endogenous retinoids in mouse embryos by HPLC with on-line solid-phase
`extraction and column-switching, Posters, HPLC 9, St. Louis, USA 1998.
`
` 3. Gundersen, TE, Ulven, SM, Blomhoff, R., Ultra Sensitive screening of retinoids in
`embryonic minute samples, items, retinoids 99, Strasbourg, France. 1999.
`
` 4. Gundersen, TE, Dahlgren, PA, Blomhoff, R., Peak Synchronised post-column injection of
`internal standards for correction of matrix ion suppression effects in electro spray ionisation.
`Poster, 23 rd Internatinal Symposium Wed chromatography, London, UK, 2000.
`
` 5. Thomassen, A, Blomhoff, R, Gundersen, T., Transfer of chromatographic methods for
`routine determination of biological samples for capillary HPLC "plug & play"?, Oral
`presentation, 15th Norwegian symposium in chromatography, 2002.
`
` 6 Sakhi, AK, Blomhoff, R, Gundersen, T., Isocratic RP-HPLC analysis of tocopherols and
`tocotrienols in plasma., Oral presentation, 15th Norwegian symposium in chromatography,
`2002.
`
` 7 Gundersen, T and Blomhoff, R., Chromatographic determination of retinoids in embryonic
`tissue from mice. Oral presentation, 15th Norwegian symposium in chromatography, 2002.
`
` 8. Gundersen TE, Invited plenary lecture “Kromatografidagene i Sandefjord”, January 2008.
`"High-throughput bioanalyse in routine. How to meet an increasing number of samples.
`
` 9. Gundersen TE, Oral presentation MareLife March, Oslo Technopole 2009
`
` 10. Gundersen TE, Oral Presentation, UCD Dublin, Human Nutrition: Where is the business?
`
`
` End.
`
`
`
`0000012
`
`

`
`       
`
`EXHIBIT 2 
`
`EXHIBIT 2
`
`0000013
`
`0000013
`
`

`
`
`
`
`
`
`
`Appendix A
`
`LC-MS(SQ) data
`
`
`
`
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 1
`
`0000014
`
`

`
`
`
`
`
`
`
`Sample P308-1
`
`Sample P308-2
`
`
`
`
`
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 2
`
`0000015
`
`

`
`
`
`
`
`
`
`
`
`
`
`Sample P308-3
`
`
`Sample P308-4
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 3
`
`0000016
`
`

`
`
`
`
`
`
`
`
`
`
`
`Sample P308-5
`
`Sample P308-6
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 4
`
`0000017
`
`

`
`
`
`
`
`
`
`
`
`
`
`
`
`Sample P308-7
`
`
`
`Sample P308-8
`
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 5
`
`0000018
`
`

`
`
`
`
`
`
`
`
`
`
`
`
`
`Sample P308-9
`
`
`Sample P308-10
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 6
`
`0000019
`
`

`
`
`
`
`
`
`
`
`
`
`
`Sample P308-11
`
`
`Sample P308-12
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 7
`
`0000020
`
`

`
`
`
`
`
`
`
`
`
`
`
`Sample P308-13
`
`Sample P308-14
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 8
`
`0000021
`
`

`
`
`
`
`
`
`
`
`
`
`
`Sample P308-15
`
`Sample P308-16
`
`
`
`Vitas as, Oslo Innovation Centre, Norway
`
`
`
`Vitas P308 Page 9
`
`0000022
`
`

`
`
`
`Appendix B
`
`MRM Data
`
`
`
`0000023
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} ‘|D.d
`
`p308-1
`p308-1
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2) ‘lD.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} ‘|D.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 524.2) ‘lD.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E52.-1 —.*—- 550.2} ‘lD.d
`
`-I-ESI MRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} ‘lD.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E26.-1 —.*—- 524.2} ‘lD.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`3.8
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000024
`
`0000024
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} ‘|‘l.d
`
`p308-2
`p308-2
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2) ‘l‘l.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} ‘|‘l.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 524.2) ‘l‘l.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E52.-1 —.*—- 550.2} ‘l‘l.d
`
`-I-ESI MRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} ‘l‘|.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E26.-1 —.*—- 524.2} ‘l‘l.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`3.8
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000025
`
`0000025
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} ‘|2.d
`
`p308-3
`p308-3
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2) ‘l2.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} ‘|2.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 524.2) ‘l2.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E52.-1 —.*—- 550.2} ‘l2.d
`
`-I-ESI MRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} ‘l2.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (E26.-1 —.*—- 524.2} ‘l2.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`3.8
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000026
`
`0000026
`
`

`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [SII‘3.-1 4+ 134.0) 123.11
`
`p308-4
`p308-4
`
`+E5| MRM Fuag=2fli.'I.D\u’ C|D@“' [ET-‘EA -> 550.2) ‘l3.d
`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [3514 4+ 134.0) 123.11
`
`+E5| MRM FIag=2fli.'I.D\I’ C|D@"‘ [$52.4 4+ 524.2) 13.11
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3524 —> 550.2) ‘l3.d
`
`-I-ESI MRM Fvag=2flfl.|J\u' C|D@"' [32E.-1 —> 134.0) ‘l3.d
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3264 —> 524.2) ‘l3.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`3.8
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000027
`
`0000027
`
`

`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [SII‘3.-1 4+ 134.0) ‘I-Ld
`
`p308-5
`p308-5
`
`+E5| MRM Fuag=2fli.'I.D\u’ C|D@“' [ET-‘EA -> 550.2) ‘I-Ld
`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [3514 4+ 134.0) ‘I-Ld
`
`+E5| MRM FIag=2fli.'I.D\I’ C|D@"‘ [$52.4 4+ 524.2) ‘l4.d
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3524 —> 550.2) ‘I-1.d
`
`-I-ESI MRM Fvag=2flfl.|J\u' C|D@"' [32E.-1 —> 134.0) ‘I-1.d
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3264 —> 524.2) ‘I-1.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`3.8
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000028
`
`0000028
`
`

`
`-I-EEI MFl|'~I FIag=2DD.[I"u' C|D@u1-[III [6T8.-4-CIDD -1?-184.CI[I[ICI)15.d
`1
`
`P308-6
`P308-6
`
`-I-EEI MRI‘-I FIag=2DD.fl‘u' C|D@GC|.fl [8T8.4[|1JD -> 55D.2fl31)15.d
`1
`
`-I-EEI MFl|'~I FIag=2DD.[I"u' C|D@u1-[III [652.-4-CIDD -1?-184.CI[I[ICI)15.d
`1
`
`1-EEI |'-'|FI|'-I FIag=2flfl.[I"u' C|D@G[I.[I [852.-4-[IUD -Cr 524.2[I31)15.d
`1
`
`-I-EEI MFl|'~I FIag=2DD.{I"u' C|D@G[I.[I [652.4[IDD -3 55D.2CI31)15.d
`1
`
`x1lII
`
`4.3
`4.2
`4.1
`
`no‘
`55
`
`1-ESI MFIM FIag=2flfl.[I‘u' C|D@|4-[I1] [£26.-4-[IUD -5} 184.0000) 15.11
`1
`
`-I-EEI MRI‘-I FIag=2DD.fl‘u' C|D@GC|.[| [826.4[|DD -3 524.2fl31)15.d
`1
`
`[I12
`
`[I14
`
`[I16
`
`[I18
`
`1
`
`1.12
`
`1.14
`
`116
`
`118
`
`2
`
`212
`
`214
`
`216
`
`218
`
`3
`
`312
`
`4.16
`4.14
`4.12
`4
`3.18
`3.16
`314
`Cuums vs. Acquisition Tune I[ni1}
`
`4.18
`
`5
`
`5.12
`
`5.14
`
`5.16
`
`5.18
`
`6
`
`6.12
`
`614
`
`616
`
`618
`
`T
`
`T12 T14
`
`T16 T18
`
`0000029
`
`0000029
`
`

`
`-I-E5| MFEII-I F|ag=2|J|].|JV CID?‘ [3]‘3.-I -> 134.0) 2.11
`
`-I-E5| MFEII-I F|ag=2|J|].|JV CID?‘ [3]‘3.-I -> 550.2) 2.11
`
`-I-E5| MFEII-I F|ag=2|J|].|JV CID?‘ [£52.-I -> 134.0) 2.11
`
`-I-ESI MFEM F|ag=2DI].IJV CID?‘ [3524 -> 52-1.2)2.d
`
`+E5I MRM Fnag=2D[I.DV CID?‘ [3524 -> 550.2) 2.cI
`
`+E5I MRM Fnag=2D[I.DV CID?‘ [E2E.4 -> ‘IE-LU) 2.cI
`
`+E5I MRM Fnag=2D[I.DV CID?‘ [E2E.4 -> 524.2) 2.cI
`
`p308-7
`p308-7
`
`4.49
`
`3.6
`
`ab
`ah
`35
`Counts us. Acquisition Tune {nil}
`
`4
`
`41
`
`-1.2
`
`4.3
`
`4.4
`
`-1.5
`
`-1.6
`
`-1.?
`
`4.3
`
`-1.9
`
`0000030
`
`0000030
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} 3.d
`
`p308-8
`p308-8
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2} 3.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} 3.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 52-1.2}3.d
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E52.-1 —.*—- 550.2} 3.d
`
`-I-ESI
`
`|'-IRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} 3.11
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E26.-1 —.*—- 52-1.2}3.d
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000031
`
`0000031
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} -1-.d
`
`p308-9
`p308-9
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2} -1-.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} -1-.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 524.2} -1-.d
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E52.-1 —.*—- 550.2}-1.d
`
`-I-ESI
`
`|'-IRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} -1.11
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E26.-1 —.*—- 524.2}-1.d
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000032
`
`0000032
`
`

`
`+ES| MFEM FIag=2[|fl.U‘U'
`
`'C|D@"‘ [BT34 -5} 134.0) 5.11
`
`p308-10
`p308-10
`
`+E5| MRM Fvag=2[Ifl.D‘U' C|D@“"" [ET-'3.-I —:=- 550.2) 5.d
`
`+E5| MRM Fvag=2[Ifl.D‘U' C|D@“"" [E524 —:=-
`
`‘I3-1.0) 5.d
`
`+ES| MFEM FIag=2[|fl.U‘U'
`
`'C|D@"‘ [3524 -5} 524.2) 5.11
`
`+E5| MRM Fvag=2[Ifl.D‘U' C|D@“"" [E524 —:=- 550.2) 5.d
`
`+ES| MFEM FIag=2[|fl.U‘U'
`
`'C|D@"‘ [3254 -5} 134.0) 5.11
`
`+ES| MFEM FIag=2[|fl.U‘U'
`
`'C|D@"‘ [3254 -5} 524.2) 5.11
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`3.13
`
`3.9
`3.3
`3.7
`Cclums vs. Acquisition Tine (nifl
`
`-1
`
`4.1
`
`4.2
`
`4.3
`
`4.4
`
`4.5
`
`-1.6
`
`4.?
`
`-1.8
`
`4.9
`
`0000033
`
`0000033
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} E.d
`
`p308-11
`p308-11
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2} E.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} E.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 52-1.2}E.d
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E52.-1 —.*—- 550.2} Ed
`
`-I-ESI
`
`|'-IRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} 13.11
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E26.-1 —.*—- 52-1.2}E.d
`
`3.5
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000034
`
`0000034
`
`

`
`p308-12
`p308-12
`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [$3.4 -c> 134.0) ?.d
`
`+E5| MRM Fuag=2fli.'I.D\u’ C|D@“' [BT34 -3? 550.2) ?.d
`
`+ES| MRM FIag=2flfl.U\I' C|D@"' [$52.4 -c> 134.0) ?.d
`
`+E5| MRM FIag=2fli.'I.D\I’ C|D@"‘ [$52.4 -c> 52-1.2)?.d
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3524 —>- 550.2) ?.d
`
`-I-ESI MRM Fvag=2flfl.|J\u' C|D@"' [S2511 —> 13-1.D)?.d
`
`+E5| MRM Fvag=2flfl.D\I’ C|D@“' [3264 —>- 52-1.2)?.d
`
`3.5
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000035
`
`0000035
`
`

`
`p308-13
`p308-13
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (EI|‘E.-1 -> 1E-1.0} E.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (ETE.-1 -> 550.2} E.d
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (E52.-1 -> 1E-1.0} E.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 52-1.2}Ed
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E52.-1 —.*—- 550.2} E.d
`
`-I-ESI
`
`|'-IRM F|ag=2DD.D\I' C|D@"' (E26.-1 —>- 1E-1.0} E.d
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E26.-1 —.*—- 524.2} Ed
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.13
`
`4.9
`
`0000036
`
`0000036
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.4 -> 184.0} ‘|E.d
`
`p308-14
`p308-14
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (EI|‘E.4 -> 550.2) ‘lE.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} ‘|E.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (352.4 -> 524.2) ‘lE.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (352.4 —.*—- 550.2} ‘lE.d
`
`-I-ESI MRM F|ag=2DD.D\I' C|D@"' (326.4 —b- 184.0} ‘lE.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (326.4 —.*—- 524.2} ‘lE.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`348
`3.|T|‘
`Counts u-5. Acquisition Tune
`
`4
`
`4.1
`
`4.2
`
`4.3
`
`4.4
`
`4.5
`
`4.13
`
`4.7
`
`4.8
`
`4.9
`
`0000037
`
`0000037
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.-1 -> 184.0} 9.d
`
`p308-15
`p308-15
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (STE.-1 -> 550.2} 9.c|
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} 9.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (E52.-1 -> 52-1.2}9.d
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E52.-1 —.*—- 550.2} 9.d
`
`-I-ESI
`
`|'-IRM F|ag=2DD.D\I' C|D@"' (E26.-1 —b- 184.0} 9.11
`
`-I-ESI MRM F|ag=2flfl.D\n’ CIDQ“ (E26.-1 —.*—- 52-1.2}9.d
`
`3.6
`
`35
`3%
`33
`Counts u-5. Acquisition Tune
`
`J
`
`-1.1
`
`-1.2
`
`-1.3
`
`4.4
`
`4.5
`
`4.13
`
`-1.7
`
`4.8
`
`4.9
`
`0000038
`
`0000038
`
`

`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (3I|‘E.4 -> 184.0} ‘|I|‘.d
`
`p308-16
`p308-16
`
`+ES| P-‘IF-IM F|ag=2flfl.D\u' CIDE” (EI|‘E.4 -> 550.2) ‘lid
`
`+ES| MRM F|ag=2flfl.lJ\I' CIDQ" (352.4 -> 184.0} ‘|I|‘.d
`
`+ES| P-‘IF-IM F|ag=2flfl.D\I' CIDQ" (352.4 -> 524.2) ‘lid
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (352.4 —.*—- 550.2} ‘l7.d
`
`-I-ESI MRM F|ag=2DD.D\I' C|D@"' (326.4 —b- 184.0} ‘l7.d
`
`-I-ESI MRM F|ag=2flfl.DV CIDQ“ (326.4 —.*—- 524.2} ‘l7.d
`
`2.8
`
`2.9
`
`3
`
`3.1
`
`3.2
`
`3.3
`
`3.4
`
`3.5
`
`35
`
`3'9
`348
`3.|T|‘
`Counts us. Acquisition Tune
`
`4
`
`4.1
`
`4.2
`
`4.3
`
`4.4
`
`4.5
`
`4.13
`
`4.7
`
`4.8
`
`4.9
`
`0000039
`
`0000039
`
`

`
`
`
`EXHIBIT 3
`
`EXHIBIT 3EXHIBIT 3
`
`
`
`
`
`00000400000040
`
`7
`
`
`
`
`
`
`
`0000040
`
`

`
`High Standard (st7)
`Time: 04:49
`
`Solvent blank after high Standard ( st7)
`Time: 05:08
`
`0000041
`
`

`
`Sample P308-9
`Time: 00:50
`Cycle time of method: 18 minutes
`
`Solvent blank after P308-9
`Time: 01:08
`
`0000042