Laboratory Corporation of America Holdings vs Quest Diagnostics Investments LLC et al.

Other: fed circuit mandate

Trial Certificate Checklist

Patent Owner's Notice of Appeal

Final Written Decision Determining All Challenged Claims Unpatentable 35 U.S.C. sec 318(a)

Hearing Transcript

Patent Owner's Demonstrative Exhibits

Petitioner's Demonstratives

Order Trial Hearing

Patent Owner's Sur-Reply

Patent Owner's Request for Oral Argument

Petitioner's Request for Oral Argument

Deposition Transcript of Patrick M. Sluss taken February 12, 2020 in IPR2019-00738

Petitioner's Reply to Patent Owner's Response

Stockl et al., Specifications for Trueness and Precision of a Reference Measurement System for Serum/Plasma 25-Hydroxyvitamin D. Analysis, Clin. Chim. Acta 408:8-13 (2009)

Declaration of Steve Lock dated August 12, 2019

Declaration of Dr. Robert Voyksner dated February 28, 2020

Declaration of Patrick M. Sluss, Ph.D. in IPR2019-00738

Deposition Transcript of Patrick M. Sluss, Ph.D. on July 27, 2020

Landmann et al., Soluable CD14 Activates Monocytic Cells Independently of Lipopolysaccharide, Infection and Immunity 66(5):2264-71 (1998)

Petitioner's Notice of Deposition of Patrick M. Sluss, PH.D. Under 37 C.F.R. section 42.53

PETITIONER UPDATED EXHIBIT LIST

Ex 3002

PETITIONER¿¿¿S OBJECTIONS TO EVIDENCE SUBMITTED WITH PATENT OWNER¿¿¿S RESPONSE

ORDER Granting Petitioner's Motion to Submit Supplemental Information

Declaration of Christopher Butler with attached Exhibit A from Zorbax HPLC Columns

Motion to Submit Supplemental Information

Declaration of Christopher Butler with attached Exhibits A and B from ASMS

Casetta, B., et al., Development of a Method for the Quantification of 1 ¿¿, 25 (OH) 2¿¿¿Vitamin D3 in Serum by Liquid Chromatography Tandem Mass Spectrometry without Derivatization. European Journal of Mass Spectrometry, 16(1), 81-89 (2010).

Patent Owner's Response

May 14, 2020 Deposition Transcript of Robert L. Fitzgerald, Ph.D.

Woods, G. N., et al., A young woman with recurrent gestational hypercalcemia and acute pancreatitis caused by CYP24A1 deficiency. Journal of Bone and Mineral Research, 31(10): 1841-1844 (2016).

Kim, S., et al., How much is too much? Two contrasting cases of excessive vitamin D supplementation. Clinica Chimica Acta, 473: 35-38 (2017).

Coburn, J. W., Metabolism and action of the hormone vitamin D: its relation to diseases of calcium homeostasis. Western Journal of Medicine, 121(1), 22 (1974).

Declaration of Patrick M. Sluss, Ph.D.

File History for U.S. Patent. No. 7,972,867.

Boyle, I.T., et al. The biological activity and metabolism of 24, 25-dihydroxyvitamin D3. Journal of Biological Chemistry 248.12: 4174-4180 (1973).

Nemere, I., Apparent nonnuclear regulation of intestinal phosphate transport: effects of 1, 25-dihydroxyvitamin D3, 24, 25-dihydroxyvitamin D3, and 25-hydroxyvitamin D3. Endocrinology 137.6:2254-2261 (1996).

Norman, A.W. From vitamin D to hormone D: fundamentals of the vitamin D endocrine system essential for good health. The American journal of clinical nutrition 88.2: 491S-499S (2008).

Higashi, T., et al.

van den Ouweland, JMW. Analysis of vitamin D metabolites by liquid chromatography-tandem mass spectrometry. TrAC Trends in Analytical Chemistry 84:117-130 (2016).

Ishimura, E., et al. Serum levels of 1, 25-dihydroxyvitamin D, 24, 25-dihydroxyvitamin D, and 25-hydroxyvitamin D in nondialyzed patients with chronic renal failure. Kidney international 55.3: 1019-1027 (1999).

Fraser, William D., et al. Vitamin D assays: past and present debates, difficulties, and developments. Calcified tissue international 92.2: 118-127 (2013).

Colston, K. W., et al. Feedback regulation of vitamin D metabolism by 1, 25-dihydroxycholecalciferol. Biochemical Journal 164.1:83-89 (1977).

Galior, K., et al. 10 years of 25-hydroxyvitamin-D testing by LC-MS/MS-trends in vitamin-D deficiency and sufficiency. Bone reports 8:268-273 (2018).

Le Goff, C., et al. Measurement of circulating 25-hydroxyvitamin D: a historical review. Practical laboratory medicine 2:1-14 (2015).

Ding, Shujing, et al., Quantitative determination of vitamin D metabolites in plasma using UHPLC-MS/MS. Analytical and bioanalytical chemistry 398.2: 779-789 (2010).

Ornoy, A., et al. 24, 25-Dihydroxyvitamin D is a metabolite of vitamin D essential for bone formation. Nature 276.5687:517-519 (1978).

Weisman, Y., et al. Serum 24, 25-dihydroxyvitamin D and 25-hydroxyvitamin D concentrations in femoral neck fracture. British medical journal 2.6146: 1196 (1978).

Niessen, W. M. A. Thermospray Ionization in Mass Spectrometry. Elsevier Reference Module Chemical, Molecular Sciences and Engineering. (2013).

Memorandum Order addressing claim construction in Civil Action No. 1:18-cv-01436 (MN) on January 14, 2020.

Patent Owner's Second Notice of Deposition of Dr. Robert L. Fitzgerald

Patent Owner's Notice of Cancellation of Deposition of Dr. Robert L. Fitzgerald

Joint Stipulation to Adjust the Scheduling Order

Patent Owner's Notice of Deposition of Dr. Robert L. Fitzgerald

Ex. 3001

Order - 37 CFR 42.123(a)

Patent Owner's Objections to Evidence

Petitioner's Updated Mandatory Notice Pursuant to 37 C.F.R. Section 42.8

Patent Owner's Updated Mandatory Notices

Scheduling Order

Decision - Instituting Inter Partes Review

ORDER Granting Patent Owner's Motion for Pro Hac Vice Admission of Thomas H. Wintner

Joint Claim Construction Chart Ex. A filed in Civil Action No. 1:18-cv-01436 (MN) on September 25, 2019

Patent Owner's Preliminary Response

File History for U.S. Patent No. 7,745,226

Patent Owner's Unopposed Motion for Pro Hac Vice Admission of Thomas H. Wintner

Declaration of Thomas H. Wintner in Support of Motion for Pro Hac Vice Admission

Patent Owner's Power of Attorney

Patent Owner's Mandatory Notices

Notice of Accord Filing Date

U.S. Patent. No. 8,101,427 to Clarke et al.

Declaration of Robert L. Fitzgerald, Ph.D., DABCC

Kamao et al., C-3 Epimerization of Vitamin D3 Metabolites and Further Metabolism of C-3 Epimers, Manuscript M311473200, JBC Papers in Press, 1-31 (2004)

Watson et al., Analysis of Vitamin D and Its Metabolites Using Thermospray Liquid Chromatography/Mass Spectrometry, Biomedical Chromatography 5:153-60 (1991)

Vogeser, Liquid Chromatography-Tandem Mass Spectrometry Application in the Clinical Laboratory, Clin.Chem. Lab. Med. 41(2):117-26 (2003)

Patent Owner Response dated April 7, 2009 for U.S. Patent No. 7,774,226

Petition for Inter Partes Review

File History for U.S. Patent. No. 8,101,427 to Clarke et al.

Voyksner and Lee, Improvements in LC/Electrospray Ion Trap Mass Spectrometry Performance Using an Off-Axis Nebulizer, Anal. Chem. 71:1441-47 (1999)

Kissmeyer and Sonne, Sensitive Analysis of 25-Dihydroxyvitamin D3 in Biological Fluids by Liquid Chromatography-Tandem Mass Spectrometry, J. Chromatography A 935:93-103 (2001)

Rainbow et al., The Analysis of Vitamin D Analogues by Atmospheric Pressure Ionization Coupled to Triple Quadrupole Mass Spectrometry, Poster No. M-045, Proceedings of the 51st ASMS Conference on Mass Spectrometry and Allied Topics, Montreal, Canada

Interview Summary dated January 28, 2009 for U.S. Patent No. 7,774,226

Office Action dated April 12, 2010 for U.S. Patent No. 7,972,867

Patent Owner Response dated July 8, 2010 for U.S. Patent No. 7,972,867

Glenville Jones and Hugh L.J. Makin, Vitamin Ds, Metabolites and Analogues, Chapter 2 in Modern Chromatographic Analysis of Vitamins, 87-153 (Leenheer, Lambert & Van Bocxlaer, eds., 3rd ed. 2000)

Declaration of Christopher Butler

Declaration of Dr. Robert Voyksner

Declaration of Patrick Gordis (for Vogeser)

National Library of Medicine, PubChem Computed Properties for Calcitriol

Zimmer et al., Comparison of Turbulent-Flow Chromatography with Automated Solid-Phase Extraction in 96-Well Plates and Liquid-Liquid Extraction Used as Plasma Sample Preparation Techniques for Liquid Chromatography-Tandem Mass Spectrometry

A. Michael Parfitt, Osteomalacia and Related Disorders,in Metabolic Bone Disease and Clinically Related Disorders, 329-96 (Aviolo, Krane, eds., 3rd ed.1997)

Trivedi et al., Effect of Four Monthly Oral Vitamin D3 (Cholecalciferol) Supplementation of Fractures and Mortality in Men and Women Living in the Community: Randomised Double Blind Controlled Trial, BMJ 326:469-74 (2003)

Leinonen et al., Liquid Chromatography/Mass Spectrometry in Anabolic Steroid Analysis ¿¿¿ Optimization and Comparison of Three Ionization Techniques, Electrospray Ionization, Atmospheric Pressure Chemical Ionization and Atmospheric Pressure Photoionization

Lagan et al., Liquid Chromatography Tandem Mass Spectrometry Applied to the Analysis of Natural and Synthetic Steroids in Environmental Waters, Analytical Letters 34(6):913-26 (2001)

Declaration of Catherine Vassilkova

Declaration of Andrew Hoofnagle, M.D., Ph.D.

Declaration of Patrick Gordis (for Watson)

Couchman, Turbulent Flow Chromatography in Bioanalysis: A Review, Biomed. Chromatography 26:892-905 (2012)

Hollis and Napoli, Improved Radioimmunoassay for Vitamin D and Its Use in Assessing Vitamin D Status, Clin. Chem. 31(11):1815-19 (1985)

Armas et al., Vitamin D2 is Much Less Effective than Vitamin D3 in Humans, J. Clin. Endocrinol. & Metab., 89:5387-91 (2004)

Kamao et al., C-3 Epimerization of Vitamin D3 Metabolites and Further Metabolism of C-3 Epimers, J. Biol. Chem. 279:15897-907 (2004)

Food and Nutrition Board, Institute of Medicine, Dietary Reference Intakes for Calcium, Magnesium, Phosphorus, Vitamin D and Fluoride 250-87 (National Academy Press 1997)

Kissmeyer et al., Determination of the Vitamin D Analog EB 1089 (Seocalcitol) in Human and Pig Serum Using Liquid Chromatography-Tandem Mass Spectrometry, J. Chromatog. B, 740:117-28 (2000)

Herbert and Johnstone, Mass Spectrometry Basics 225-35, 245-52, 261-68, and 413-15 (CRC Press LLC, 2002)

Fitzgerald et al., Broad Spectrum Drug Identification Directly from Urine, Using Liquid Chromatography-Tandem Mass Spectrometry, Clin. Chem. 45:1224-34 (1999)

Fitzgerald et al., Comparison of an Ion Trap and a Quadrupole Mass Spectrometer Using Diazepam as a Model Compound, J. Analytical Toxicology 21:445-50 (1997)

Ma and Kim, Determination of Steroids by Liquid Chromatography/Mass Spectrometry, J. Am. Soc. Mass Spectrom. 8:1010-20 (1997)

Fred W. McLafferty & Frantisek Turecek, Interpretation of Mass Spectra 349 (4th ed. 1993)

Francis A. Carey, Stereochemistry,in Organic Chemistry 259-301 (McGraw-Hill, 4th ed. 2000)

Davankov, Analytical Chiral Separation Methods (IUPAC Recommendations 1997), Pure and Applied Chemistry 69:1467-74 (1997)

Mac-Mod Zorbax HPLC Columns Product Bulletin

Declaration of Dr. Russell Grant

Power of Attorney