Analytical comparability of a human IgG1 from different manufacturing sites after cell line switch and process changes: A case study Dr. Margit Jeschke Head Analytical R&D Novartis Biologics www.diahome.org Disclaimer The views and opinions expressed in the following PowerPoint slides are those of the individual presenter and should not be attributed to Drug Information Association, Inc. (“DIA”), its directors, officers, employees, volunteers, members, chapters, councils, Special Interest Area Communities or affiliates, or any organization with which the presenter is employed or affiliated. These PowerPoint slides are the intellectual property of the individual presenter and are protected under the copyright laws of the United States of America and other countries. Used by permission. All rights reserved. Drug Information Association, DIA and DIA logo are registered trademarks or trademarks of Drug Information Association Inc. All other trademarks are the property of their respective owners. www.diahome.org Outline Introduction Molecular Challenges with mAb1NVS Results • Purification Process Performance • Physicochemical tests • Biological characterization • Accelerated Stabilty Study • Preclinical & PK/PD Summary Conclusions & Discussion Acknowledgements 3 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Drug substance Drug product Overview mAb1NVS Drug Substance & Product PhII hPoC DP 50mg Lyo i.v. Prod. Site Cell line Qualities PhIII Market 150mg Lyo i.v. & s.c Basel PharmOps SP2/0 CHO Type A Type B Type C Type D Type E PoC quality PoC quality Prototype Prototype Final market quality Major change Site 4 | 2009 DIA Comparability | Comparability | Jeschke M | 4-Feb-09 Launch site mAb1NVS Manufacturing Changes Changes in drug substance manufacturing process for phase I/II clinical development: • production cell line (Sp2/0 to CHO) • manufacturing process • manufacturing site • scale-up 5 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Summary of Changes Cell Process 2 Process 3 Process 4 Process 5 Sp2/0 Sp2/0 CHO CHO Site Scale 3’000L 3’000L 1’500L USP hTransferrin: Celliance hTransferrin: Millipore w/ yeastolate no transferrin Harvest Centrifugation Centrifugation Microfiltration + microfiltration + microfiltration AEX CEX AEX CEX Nanofiltration at the end of purification at the end of purification DSP 6 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 13’000L w/ yeastolate no transferrin Centrifugation + microfiltration selective red. selective red. CEXAEX CEXAEX at the end of at early state purification Process 1: SP2/0 Molecular Challenges X-ray structure of the mAb1NVS Fab fragment (2.80Å resolution) H-CDR3 H-CDR1 Heavy chain (HC) H-CDR2 Light chain (LC) LC-Cys-SH L-CDR2 L-CDR1 L-CDR3 Free thiol group required for biological activity 7 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Medium dependent biological activity human IgG active mAB Titer (mg/L) 300 Medium Komponenten D-Glucose 200 mg/l 2000 4500 240nM 50uM 0.25 225nM Nickel(II) Chloride 17% 10% active 108% Zinc sulfate (ZnSO4-7H2O) Glutathione Reduced 0 2 mg/l Fe(III)citrate 102% 1 Prod. Cupric sulfate (CuSO4-5H2O) 46% 100 A 3 medium: A 2055 4 5 2071 Prod. Mercaptoethanol L-Cystine-2HCl 1 50uM 65.15 5 50uM 325.75 cysteinylation interferes with antigen binding production of biologically active antibody: A: fermentation of active mAb, e.g. by reduction of the cystine concentration B: modulation of activity during protein purification by treatment with reducing agents 8 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Xolair 3‘/ 85°C - IA Xolair 3‘/ 85°C 10‘/ 85°C - IA 10‘/ 85°C 2‘ / 85°C 1‘ / 85°C 2‘ / 60°C not heated 3‘/85°C prestained Marker More mAb1NVS idiosyncrasies By- and degradation products by SDS-PAGE (non-reducing) Intact antibody IA = treated with Iodoacetamide Disulfide scrambling 9 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Overview mAb1NVS comparability exercise Comparability Comparison of post-change product to pre-change product at different levels: Safety and efficacy Not done PK/PD PK/PD in healthy volunteers Preclinical Tox studies in monkeys Tissue crossreactivity studies Biological characterization Physicochemical level 10 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Target binding & potency Fc Receptor binding Comprehensive analytical characterization Batches for analytical comparability Sp2/0 P2 Sp2/0 P3 SP2/0-S06 SP2/0-S07 CHO P4 CHO P5 CHO-B07 CHO-S07 Two representative drug substance batches from each process were chosen to assess: the process performance (incl. IPC) physicochemical properties biological characterization: antigen binding, Fc receptor binding, and potency accelerated stability (6 months) 11 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Outline Introduction Molecular Challenges with mAb1NVS Results • Purification Process Performance • Physicochemical tests • Biological characterization • Accelerated Stabilty Study • Preclinical & PK/PD Summary Conclusions & Discussion Acknowledgements 12 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Purification Process Performance Process performance - ProtA, HCP, DNA and yields: • The single step efficiency is different • Overall removal successful for all process related impurities • Single step yields are different 13 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Physicochemical characterization Release tests Comparison of release data for mAb1NVS drug substance batches (CHO processes) Test Requirement CHO-B07 A CHO-B07 B CHO-B07 C Appearance of the solution: Turbidity pH value Assay by SEC [mg/ml] free SH-groups [Mol/Mol] Impurity by SDSPAGE (reducing) Related substances by SEC Clear to opalescent Opalescent Opalescent Clear Inhibition of IL-x release CHO HCPs Protein A ELISA Residual DNA MLT BET CHO-B07 D CHO-B07 E CHO-B07 F CHO-S07 A CHO-S07 B 60.0 6.2 64.9 6.3 64.6 6.0 66.0 Slightly opalescent 6.1 66.6 ≥ 2.0 2.6 2.6 2.5 2.5 2.5 2.6 2.3 2.2 Sum of impurities ≤ 0.3 % 5.0 % aggregates: ≤ 5.0 % 0.3 % fragments: ≤ 5.0 % <0.1% <0.25 % <0.25 % <0.25 % 0.5 % 0.4 % 1.0% 1.0% 0.4 % <0.1% 0.4 % <0.1% 0.4 % <0.1% 0.5 % <0.1% 0.5 % 0.3% 0.3 % 0.0 % 0.2 % 0.0 % 80% - 125 % 97 % 96 % 108 % 99 % 98 % 99 % 94% 92 % Not yet defined ≤ 5 [ng/mg AIN457] ≤ 8.3 pg/mg AIN457 ≤ 10 [cfu/ml] ≤ 0.1 [EU/mg] n.p. <1 n.p. n.p. < 0.0033 < 1 ng/mg <1 <2 <1 < 0.0033 < 1 ng/mg <1 <2 <1 < 0.0033 < 1 ng/mg <1 <2 <1 < 0.0033 < 1 ng/mg <1 <2 1 < 0.0033 < 1 ng/mg <1 <2 <1 < 0.0033 < 1 ng/mg <1 <2 0 < 0.01 < 1 ng/mg. <1 <2 0 0.02 5.5 – 6.5 14 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Slightly opalescent 6.2 65.2 Slightly opalescent 6.1 64.4 Slightly opalescent 6.1 71.6 Slightly opalescent 6.3 69.4 Physicochemical characterization Protein identity – reduced Pep Map and Q-ToF MS • Nearly all (96%/99%) peptides were identified by MS • CHO/CHO: Comparable pattern of peaks (no new peaks, no peak missing) • CHO/Sp2/0: Additional peaks for C-terminal variants in the CHO material + different peaks for the carbohydrate variants HC158-215 HC66-143 LC41-108 HC299 -327+ N -glycans HC233-256 HC371-424 LC128 -146 HC233-258 LC1-40 HC259-284 LC109 -127 HC403-419 HC381-402 HC425-449 HC285-298, HC44-58 LC171 -184 HC132 -143 HC371 -380 HC351 -370 HC144-157 LC192-208 HC450-455 HC450-456 HC337-344 HC66-76 HC450 -457 LC151-170 HC59-65 LC147-150 LC209-215 HC420-424 200 HC345-348 LC185 -189 HC224-228 400 HC158-220 HC1-43 CHO-B07 600 HC277-143, HC77 -131 ens. 0 20 40 60 80 100 120 Q-ToF MS: mass differences according to the carbohydrate variations 15 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 140 Time [min] Physicochemical characterization Carbohydrate heterogeneity M8 M7 bG2 M8 M7 bG2+Gal SP2/0-S07 bG2 50 1,6 / 1,3 hG0M6 100 M5 bG1ΔGlcNAc bG0ΔGlcNAc 150 bG0 0 Intens.40 M6 50 1,6 bG1 100 CHO-S07 1,3 bG1 M6 bG0ΔFuc 150 M5 1,6/1,3 bG1ΔFuc bG0 Intens. 1,3 bG1 1,6 bG1 Quantification: NP-HPLC Q-TOF Analysis (full size mAb) Peptide mapping of N-Glycan containing peptides 0 40 16 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 50 60 70 80 90 100 110 Time [min] Physicochemical characterization Carbohydrate heterogeneity 25 Sp2/0-S06 Sp2/0-S07 20 CHO-B07 CHO-S07 15 10 M8 bG2+Gal Man7 bG2 1,3/ 1,6 hG0M6 bG2-[Fuc] Man6 1,3 bG1 1,6 bG1 1,3/1,6 bG1-[Fuc] 1,3/1,6 bG1-[Fuc] bG1-[GlcNAc] Man5 bG0 bG0-[GlcNAc] 0 bG0-[Fuc] 5 Only CHO material contains bG0/1/2 ΔFucose CHO material contains less high mannose forms Only Sp2/0 material contains bG0 ΔGlcNAc, bG1 ΔGlcNAc 17 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Physicochemical characterization Protein impurities - SEC Monomer 9.0 8.0 7.0 Aggregate – AP1 6.0 Degradation products 5.0 4.0 CHO --B07 4 3.0 Sp2/0 - S06 3 2.0 2 CHO --S07 1.0 0.0 1 Sp2/0 - S07 min 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 Same impurity profile 18 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 25.0 26.0 27.0 27.7 Physicochemical characterization Protein impurities - SDS-PAGE non-red. / silver stain 072204 CHOCHO-S07 072203 062101 Sp2/0 071206 071205 071204 071203 CHOCHO-B07 071202 CHOCHO-S07 Unstained MWM CHOCHO-B07 blocked/non-reduced 40-500 KDa non blocked/non-reduced 500 KDa 290 KDa 240 KDa HHLL 160 KDa HHL 116 KDa HH 97 KDa HL 66 KDa 55 KDa 40 KDa 19 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 H Physicochemical characterization Charge heterogenity – Comparison by HPLC-CEX CEX (native and after treatment with carboxypeptidase B): • All batches show the rank order of abundance of charge isoforms 00 > K0 > KK • Same charged isoforms CHO/CHO; different charged isoforms Sp2/0/CHO 2,000 1,500 1,875 Inhbit = Off 1,375 mAU 0K 0K 1,750 1,625 1,250 1,500 1,125 1,375 1,000 1,250 875 Acidic variants 1,125 Acidic variants 750 Additional charge variant 1,000 1K 875 625 4 500 375 3 2K 750 Sp2/0- S06 625 500 Sp2/0- S07 375 250 2 250 CHO-B07 125 125 0 1 CHO-S07 0 -200 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 20 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 18.0 19.0 -200 20.08.0 21.09.0 22.0 10.0 23.0 11.0 24.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 2 Physicochemical characterization Higher order structure – Circular dichroism spectroscopy Far UV Near UV CD spectra of the four mAb1NVS batches are comparable 21 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Free SH group – calculated activity Cystamine labeling / CEX 500 450 WVL:220 nm 40.0 400 37.5 active 50% 35.0 350 32.5 active 30.0 300 27.5 25.0 250 22.5 20.0 200 inactive 17.5 Sp2/0- S07 15.0 150 12.5 CHO-B07 - 10.0 100 7.5 CHO-S07 - 5.0 50 4 3 2 1 min 1.4 20.1 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 30.5 31.0 31.5 32.0 Sp2/0- S06 32.6 min -20 0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 30.0 32.0 34.0 36.0 38.0 40.0 42.0 Theoretical activity (%) of mAb1NVS drug substance batches based on cystamine derivatization Sp2/0- S06 Total calculated activity [%] 22 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 96.7 Sp2/0-S07 CHO-B07 CHO-S07 97.3 96.7 97.8 45.0 Biological characterization Bioassys Affinity (Biacore) Binding characteristics (kon and binding constant) to human target IL-x kon [105 M-1 s-1] koff [10-5 s-1] KD [10-10 M] Sp2/0-S06 062101 Sp2/0-S07 072105 CHO-B07 071202 CHO-S07 072203 1.3 ± 0.0 2.3 ± 0.4 1.8 ± 0.3 1.3 ± 0.0 2.1 ± 0.1 1.6 ± 0.1 1.3 ± 0.0 2.4 ± 0.1 1.9 ± 0.1 1.3 ± 0.0 2.0 ± 0.1 1.6 ± 0.1 Comparison of Potency: Inhibition of IL-x release target cells Relative biological activity [%] 23 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Sp2/0-S06 062101 99 Sp2/0-S07 072105 96 CHO-B07 071202 100 CHO-S07 072203 94 Biological characterization Fc Receptor binding Biacore: • comparable high affinity binding to target • increased affinity to FcγRIIIa and FcγRIIIb for the CHO-B07 material KD values for interactions of mAb1NVS with Fc receptors Sp2/0-06 Sp2/0-07 CHO-B07 CHO-S07 FcγRIa 20.1 nM 21.2 nM 22.0 nM 24.9 nM FcγRIIa 7.4 µM 7.7 µM 6.7 µM 7.5 µM FcγRIIIa (F158) 13.5 µM 13.5 µM 8.6 µM 14.3 µM FcγRIIIa (V158) 6.8 µM 6.1 µM 4.3 µM 8.1 µM FcγRIIIb 28.9 µM 29.5 µM 18.0 µM 30.3 µM 24 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Physicochemical and Biological characterization Comparability - summary Analytical technique Requirement Result CHO/CHO Sp2/0/CHO Non-reduced molecular weight by Q-ToF MS Same molecular mass Reduced Lys-C Pep Map Same peptides Carbohydrates HPLC of enzymatically cleaved and derivatized glycan residues Same carbohydrates Bioactivity Inhibition of IL-x release Same inhibition Affinity constants for binding to target (Biacore) Same binding constants Binding to soluble Fcreceptors Biacore Same binding constants Identity 25 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Physicochemical characterization Comparability - summary Analytical technique Requirement Result CHO/CHO Protein impurities Sp2/0/CHO SDS-PAGE (reduced and non-reduced) with silver staining Comparable band pattern + no additional bands HPLC-SEC Same impurity profile and no new component above LOQ Soluble aggregates by DLS Same size distribution and average hydrodynamic radii SLS/MALLS Same average molecular mass/ same distribution 26 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Physicochemical characterization Comparability - summary Analytical technique Requirement Result CHO/CHO Charge heterogenity Free SH-group Higher order structure Sp2/0/CHO CEX undigested Same charge variants CEX digested Same charge variants IEF Same isoelectric points Cystamine CEX Theoretical activity ≥ 90% for each batch Ellman’s assay 2.2 to 2.8 Mol/Mol CD spectroscopy Same spectra 27 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Accelerated stability study Program and analytical Tests Short term stability program storage condition <-60°C (for comparison) 25°C / 60% RH 40°C/75% RH 6 weeks 3 months 6 months x - x x x x x x Test performed for the head to head stability: • SDS-PAGE • SEC – Assay and Purity • CEX • Free SH groups • Appearance / Color / pH • Bioassay 28 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Accelerated stability study Stability results 25°C - SEC Aggregates Fragments 4 2.5 3.5 2 3 2.5 1.5 2 1 1.5 1 0.5 0.5 0 0 initial 1.5 months 3 months 6 months initial 1.5 months SP2/0-S06 – SP2/0-S07 – CHO-B07 – CHO-S07 29 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 3 months 6 months Accelerated stability study AP3 20.0 18.0 071202 -CHO-B07 monomer 22.0 072203 -CHO-S07 WVL:210 nm 072105 Sp2/0-S07 25.0 mAb1NVS reference Overlay of SEC chromatograms – 3M 25°C (062101 Sp2/0-S06) Stability results 25°C – SEC & red. SDS-PAGE MWM [kDa] DP1 16.0 1.5% 2.0% 14.0 12.0 heavy chain DP3 200 116 97 66 55 10.0 8.0 4 37 31 071202 / CHO-B07 light chain 062101 / Sp2/0-S06 6.0 3 22 4.0 072105 / Sp2/0-S07 14 2 2.0 072203 / CHO-S07 6 1 min -1.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 26.0 4 27.0 6 Months 25°C 30 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Accelerated stability study Stability results 3 months 25°C – CEX 1 - DM_080318_01 #11 [modified by mezzodo1] 0K 1,200 1,100 Basic variants Acidic variants 1,000 900 800 700 600 500 400 Sp2/0 - S06 / 062101 300 4 200 3 CHO -S07 / 072203 100 2 CHO -B07 / 071202 1 Sp2/0 - 07 / 072105 min -30 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 samples stored for 3 months at 25°C/60% RH 31 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 25.0 26.0 Accelerated stability study Stability results 25°C – Cell based functional bioassay 110 Bioassay Storage time [months] initial Storage at 25°C / 60% RH 1.5 3 6 Storage at 40°C / 75% RH 1.5 3 6 Sp2/0S06 Sp2/0S07 CHOB07 CHOS07 91 100 96 94 100 90 80 74 76 55 95 85 68 95 92 85 105 103 88 70 60 50 62 45 26 66 45 21 76 58 62 94 71 65 40 initial 1.5 months 3 months 6 months SP2/0-S06 – SP2/0-S07 CHO-B07 – CHO-S07 32 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Comparability – Summary & Conclusion Process performance - ProtA, HCP and DNA: • The single step efficiencies are different especially for DNA • Overall removal successful for all processes Release testing: • All release requirements and additional comparability requirements met Stability testing: • no critical observation for any stability parameter tested Additional testing: • CHO-CHO: differences in amount of carbohydrates • CHO-Sp2/0: • Differences in amount and kind of carbohydrates • Differences in binding strength to soluble Fc receptors • Variations in charge heterogeneity Analysis of the materials (CHO-CHO and CHO-Sp2/0) shows some differences 33 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Comparability – Summary Overview Differences Sp2/0 process CHO CHO Charge variants - Δ Lys – Gly variant - remaining charge variant after Lys digest Carbohydrates - non-fucosylated variants Higher amounts of ΔFucose variant Binging to soluble FcRIIIb receptor - slightly higher binding affinity Processes Different efficiency in process impurity removal Slightly lower efficiency in process impurity removal Clinical studies PhI (Ph II) (Ph II) Tox studies No immunogenicity was detected No immunogenicity was detected No immunogenicity detected PK/PD x x x 34 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Additional studies Tissue crossreactivity studies • Comparison of positive staining from human tissues treated with SP2/0 and CHO derived mAB1NVS In vivo repeated dose toxicity studies • 4 week intravenous toxicity studies in cynomolgus monkeys (incl. 8 or 10 weeks recovery) • All serum samples were analyzed for mAB1NVS by target-based and anti-idiotype competitive ELISA PK and TK in cynomolgus monkey • pharmacokinetic single dose PK and 4 weeks tox studies in cynomolgus monkeys (iv dosing) with SP2/0-derived material and CHO-derived material) 35 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Single dose cyno PK study (10 mg/kg i.v.) Comparison of PK profiles of CHO- and Sp2/0-derived mAB1NVS Comparison of target-based and anti-idiotype ELISA assays PK - CHO cell Animal 1-Anti ID Animal 1-Target 350 Animal 2 -Anti-ID 250 Animal 2 -Target 150 50 concentartion (ug/ml) 450 450 Concentration (ug/mL) PK - SP2/O cell Animal 3-Anti ID Animal 3 -Target Animal 4 -Anti-ID Animal 4-Target 400 350 300 250 200 150 100 50 0 -50 1 2 3 4 7 10 14 21 28 36 42 Time after injection in days 0.003 1 2 3 4 7 10 14 21 28 36 42 Time after injection in days Similar profiles obtained with CHO- and Sp2/0-derived mAB1NVS 36 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Toxicokinetics 4 weeks cyno tox studies (3M + 3F /group) (SP2/0): doses: 0, 10, 30, 100 mg/kg (CHO): doses: 0, 15, 50, 150 mg/kg 8 (SP2/0) or 10 (CHO) week recovery iv iv iv D1 D8 D15 D22 D29 TK profile 37 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 iv 2M+2F (dose groups 0 and 100/150 mg/kg) TK profile Toxicokinetics 10000 10000 mAb1NVS (ug/mL) SP2/0 Recovery females 1000 CHO Animal # 404 (M) Animal # 405 (M) 1000 Animal # 454 (F) Animal # 455 (F) 100 recovery males 100 Time (h) t1/2, males = 13.7 days t1/2, females = 20.0 days 38 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 1461 1369 1277 1186 1096 1004 912 821 731 639 547 456 366 274 182 91 10 0 mAb1NVS concentration (µg/mL) Mean concentrations of mAb1NVS in cynomolgus serum and recovery phase 0 200 400 600 800 1000 1200 1400 1600 1800 Time (hours) t1/2, males = 11.6 days t1/2, females = 14.6 days 2000 Are they comparable ??? „comparable does not mean identical“ FDA. August 16, 2004 (Vol 69, # 157, Pages 50386ff); Scientific Considerations Related to Developing Follow-on Protein Products 39 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 “During characterization of the drug substance a change to the glycosylation pattern was observed during the comparability exercise. Although it was demonstrated, that the difference in glycosylation obviously had no effect on the biological function, one can not exclude that there might be an immunogenic potential of the new glycans, which were identified in the CHO-derived material and therefore glycosylation should currently be part of the release specifications in order to demonstrate batch to batch consistency.” - Paul-Ehrlich-Institute (2008) 40 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Lessons learned In-depth analytical characterization and understanding of critical quality attributes is key to successful comparability Perform risk assessment for planned changes and discuss implications upfront Release Specs alone are inadequate to show no impact of change. Perform side-by-side analysis whenever possible Keep retain samples of all batches and as long as possible overload IEF / SDS-PAGE or silver stain to see low amount impurities. Use exact same samples used for IPC analysis Same test methods – otherwise describe differences Explain differences well (incl. variation of methods used) In the discussion of differences consider intended purpose 41 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 ACKNOWLEDGEMENTS Manuela Schärpf Christoph Bächler Cornelius Fritsch Georg Hölzl Steffen Pahlich Iso Lengwiler Manuel Diez Marc Hassel Hui Zhao Gerard Bruin Markus Blümel Michaela Dehio Yuan Xu 42 | 2009 DIA Comparability | Jeschke M | 4-Feb-09 Novartis Biologics, Basel, Switzerland Novartis Basel 43 | 2009 DIA Comparability | Jeschke M | 4-Feb-09