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Table 2.6.3.2: Primary Pharmacodynamics

Test Article: Asunaprevir (BMS-650032) In Vitro

Type of Study Test System Noteworthy Findings Testing

Facility Report No. Location in Dossier Anti-HCV NS3

protease activity Measured activity against purified recombinant HCV NS3/4A protease by monitoring the cleavage of a FRET-labeled peptide substrate loosely based on a cleavage site of authentic polyprotein

ASV exhibited IC50 values of 0.3 to 320 nM against purified NS3/4A protease enzyme complexes generated from 9 strains representative of each of the 6 major genotypes. In a survey of 3 strains representative of GT-1, the compound exhibited IC50 values ranging from 0.3 to 1.8 nM. GT-2 and GT-3 representatives were least susceptible (IC50 values ranging from 15 to 320 nM). GT-4, GT-5, and GT-6 representatives exhibited IC50 values ranging from 0.9 to 1.7 nM.

BMS 930023123 CTD 4.2.1.1.1

Selectivity for HCV

NS3 protease Measured activity of respective purified recombinant proteases by monitoring the cleavage of their respective substrates

ASV exerted minimal to no activity against the closely related viral serine protease, GBV-B NS3 protease, and a panel of 10 human serine and cysteine proteases.

BMS 930023123 CTD 4.2.1.1.1

Anti-HCV activity in

cell culture Measured luciferase or FRET signals in HuH-7 cells either constitutively or transiently expressing HCV (hybrid) replicons

ASV exhibited EC50 values ranging from 1 to 230 nM against HCV replicons representing GT-1a, GT-1b, and GT-2a. Against GT-2b and GT-3a NS3 protease replicon hybrids, ASV exhibited EC50 values of 0.48 μM and 1.2 μM, respectively. Against genotype 4 NS3 protease replicon hybrids, ASV exhibited EC50 values ranging from 1.8 to 7.6 nM.

BMS 930023123

930057191 CTD 4.2.1.1.1 CTD 4.2.1.1.6

Human serum effect on

anti-HCV potency Measured HCV RNA replication in HuH-7 cells constitutively expressing subgenomic HCV replicons

ASV activity was moderately attenuated in the presence of 40% human serum (6.5-fold increase in EC50 value against a replicon representing genotype subtype 1b).

BMS 930023123 CTD 4.2.1.1.1

Cytotoxicity Proliferation assays against a panel

of cell lines CC50 values ranging from 11 to 38 μM were obtained against 6 human cell lines derived from T-cells, liver, lung, cervix, and kidney cells.

BMS 930023123 CTD 4.2.1.1.1

Anti-HCV viral

activity in cell culture Measured HCV RNA replication in HuH-7 cells infected with a full length infectious virus construct

ASV exhibited an EC50 value of 39 nM against HCV infectious virus representing a genotype 2a strain.

BMS 930023123 CTD 4.2.1.1.1

Table 2.6.3.2: Primary Pharmacodynamics

Test Article: Asunaprevir (BMS-650032) In Vitro

Type of Study Test System Noteworthy Findings Testing

Facility Report No. Location in Dossier Selectivity for HCV in

cell culture Antiviral assays performed using 4

different RNA viruses ASV is a selective inhibitor of HCV genotype 1 RNA replication (EC50 1.2 to 4 nM);

showed no significant activity against BVDV (EC50 = 12 μM), HIV (EC50 = 14 μM), HRV (EC50 > 100 μM) or HCoV (EC50 > 100 μM).

BMS 930023123 CTD 4.2.1.1.1

Mode of action against

the HCV NS3 protease Characterized activity using purified recombinant HCV NS3/4A protease complex and monitoring the cleavage of a FRET-labeled peptide substrate

ASV competitively inhibited the binding of substrate to NS3/4A protease complex in a continuous FRET assay. ASV bound directly and reversibly to the protease, Ki 0.24 to 1.0 nM, depending on the genotype strain employed.

BMS 930023124 CTD 4.2.1.1.2

Resistance Cell culture passage of HCV replicons in the presence of ASV;

luciferase activity monitored in HuH-7 cells either constitutively or transiently expressing HCV replicon variants

HCV GT-1a and GT-1b replicons with reduced susceptibility to ASV were selected.

In genotype 1a replicons, the following substitutions were observed in the NS3 protease domain: T40A, Q41E, V51A, R62K, D79E, T95A, I114V, R123G, R155K, D168G, I170T, N174Y, L175P, G176E. NS3 protease substitution R155K, when introduced into recombinant HCV replicons, conferred resistance to ASV in a cell-based assay. The level of resistance was moderate for this substitution (21-fold loss in EC50 value compared with parent GT-1a replicon). In GT-1b replicons, the following substitutions were observed in the NS3 protease domain:

Q41R, Q80R, Q86R, P89L, Y105C, D168A/G/H/V/Y, E173G, and E176G. NS3 protease substitution D168V, when introduced into recombinant HCV replicons, conferred resistance to ASV in a cell-based assay. The level of resistance was high for this substitution (280-fold loss in EC50 value compared with parent GT-1b replicon).

BMS 930023124

930035268 CTD 4.2.1.1.2 CTD 4.2.1.1.3

Table 2.6.3.2: Primary Pharmacodynamics

Test Article: Asunaprevir (BMS-650032) In Vitro

Type of Study Test System Noteworthy Findings Testing

Facility Report No. Location in Dossier Cross-resistance HCV replicon transient luciferase

cell-based assays to monitor activity against NS3 protease clinical resistance variants

HCV replicons conferring resistance to inhibitors such as boceprevir and telaprevir were examined for their susceptibility to ASV inhibition. Against GT-1a replicons carrying NS3 protease substitutions at amino acid positions V36 (V36A/L/M), T54 (T54A/S), R155 (R155K), and V36-R155 (V36M-R155K), ASV exhibited no/minimal to moderate cross-resistance with EC50 values ranging from 0.33 to 42 nM (parent GT-1a replicon EC50 = 0.76 nM). Against GT-1b replicons carrying NS3 protease substitutions at amino acid positions A156 (A156S/T/V), demonstrated low to moderate resistance with EC50 values of 5.4 to 17 nM (parent GT-1b replicon EC50 = 0.86 nM).

BMS 930057191 CTD 4.2.1.1.6

Combination studies HCV replicon cell-based assay in HuH-7 cells to monitor effects of combining HCV inhibitors of different mechanisms

Combinations of ASV with other classes of HCV inhibitors including interferons alfa and lambda, ribavirin, NS5A,

showed additive to synergistic antiviral activity in vitro, with no antagonistic antiviral activity.

No apparent enhancement of cytotoxicity was seen. Treatment of HCV GT-1a replicons and HCV GT-1a replicons carrying the NS3 substitution R155K with a combination of ASV, daclatasvir, and interferon-alfa similarly suppressed HCV RNA replication.

BMS 930023123

930029019 930033004 930057191

CTD 4.2.1.1.1 CTD 4.2.1.1.4 CTD 4.2.1.1.5 CTD 4.2.1.1.6

Abbreviations: ASV = asunaprevir or BMS-650032, BVDV = bovine viral diarrhea virus, CC50 = concentration of drug to kill 50% of cells, EC50 = 50% effective concentration in reducing viral replication, FRET = fluorescence resonance energy transfer, GBV-B = GB virus B, GT = genotype, HIV = human immunodeficiency virus, HRV = human rhinovirus, HCoV = human coronavirus, HCV = hepatitis C virus, IC50 = 50% inhibitory concentration, Ki = inhibition constant, μM = micromolar, nM = nanomolar, NS3 = nonstructural protein 3, NS3/4A = nonstructural protein 3/nonstructural protein 4A, RNA = ribonucleic acid

3 副次的薬理試験

Table 2.6.3.3: Secondary Pharmacodynamics

Test Article: Asunaprevir (BMS-650032)

In Vitro Test System Noteworthy Findings Testing

Facility Report No. Location in Dossier Type of Study

Mode of action on the

IFNβ response Cardif proteolytic cleavage assay and IFNβ luciferase reporter assay in 293T cells.

ASV inhibited proteolytic cleavage of Cardif by HCV NS3/4A protease, as visualized by Western immunoblotting. Cleavage of Cardif by the presence of NS3/4A protease subsequently leads to suppression of transcription of IFN genes; addition of ASV restores transcription of IFN genes in a dose-dependent manner.

BMS 930023124 CTD 4.2.1.1.2

Abbreviations: ASV = asunaprevir or BMS-650032, Cardif = caspase recruitment domain adaptor inducing IFNβ, HCV = hepatitis C virus, IFN = interferon, IFNβ = interferon-beta, NS3/4A = nonstructural protein 3/nonstructural protein 4A.

4 安全性薬理試験

Table 2.6.3.4: Safety Pharmacology

Test Article: Asunaprevir (BMS-650032) Organ Systems

Evaluated Species/

Strain Method of

Administration Doses (mg/kg)

Gender and No.

per Group Noteworthy Findings GLP

Compliance

Study No./

Document Control Receptors, No.

enzymes, ion channels, and transporters

Human, rat, guinea

pig In vitro 10 μM

(7.5 μg/mL) NA BMS-650032 did not exhibit clear selectivity for any of the 37 targets tested (biochemical, enzyme activity, and ligand binding assays).

nonGLP DT07078/

930022950

Cardiovascular,

Electrophysiology Human/HEK 293 cells and hERG channel

In vitro 10, 30 μM

(7.5, 22.5 μg/mL)

NA ≥ 10 μM: Mild-moderate inhibition of hERG potassium currents (8.2-20.6% vs pretest); IC50 > 30 μM

nonGLP DT07089/

930023617

Human/HEK 293 cells and sodium channel (SCN5A)

In vitro 10, 30 μM

(7.5, 22.5 μg/mL)

NA ≥ 10 μM: Mild-moderate inhibition of sodium currents (26.6-65.9% vs pretest at 1 Hz stimulation frequency and 29.8-71.6%

vs pretest at 4 Hz)

nonGLP DT07089/

930023617

Human/HEK 293 cells and L-type calcium channel

In vitro 30 μM

(22.5 μg/mL) NA 30 μM: Mild-moderate inhibition of L-type

calcium (Cav 1.2) (18.3% vs pretest). nonGLP DT07089/

930023617

Rabbit/cardiac

Purkinje fiber In vitro 3, 10, 30 μM (2.2, 7.5, 22.5 μg/mL)

NA ≤ 30 μM: No BMS-650032-related findings. nonGLP DT07089/

930023617

Dog/Beagle

(telemetered) Oral (capsule) 0, 100

(single dose) 3 M, 3 F 100 mg/kg: Unformed and/or liquid stool in 2 M and 2 F 1 day post dose, bloody stool on Day 6 and unformed/mucoid stool on Days 6-9 in 1 M.

Maximum BMS-650032 plasma

concentration (4 h post dose): 43.68 μg/mL (M); 70.36 μg/mL (F).

nonGLP DS07001/

930021202

Table 2.6.3.4: Safety Pharmacology

Test Article: Asunaprevir (BMS-650032) Organ Systems

Evaluated Species/

Strain Method of

Administration Doses (mg/kg)

Gender and No.

per Group Noteworthy Findings GLP

Compliance

Study No./

Document Control Cardiovascular, No.

Electrophysiology Rabbit/

isolated heart In vitro 0, 10 μM

(0, 7.5 μg/mL) 2 or 3 F 10 μM: No BMS-650032-related findings. nonGLP DT07013/

930023505

Rabbit/NZW IV infusion 0, 3, 10, 30 3 M ≥ 3 mg/kg: Minimal dose-dependent increases (10-24% vs pretreatment) in blood pressure.

Plasma BMS-650032 concentrations 15-180 μg/mL.

nonGLP DT06116/

930023510

Respiratory and

Neurologic Mouse/

Crl:CD1 (ICR) Oral (gavage) 0, 200, 600, 2000 (single dose)

5 M, 5 F ≤ 2000 mg/kg: No respiratory or CNS

effects. GLP DM07027/

930024006

Rat/Crl:CD (SD) Oral (gavage) 0, 200, 600, 2000 (single dose)

5 M, 5 F ≤ 2000 mg/kg: No respiratory or CNS

effects. GLP DM07028/

930023864

Rat/Crl:CD (SD) Oral (gavage) 0, 30, 100, 600

(1 month) 15 M, 15 F ≤ 600 mg/kg: No noteworthy findings.

Cmax values at 30, 100, and 600 mg/kg were up to 0.306, 13.7, and 43.4 μg/mL.

GLP DM07024/

930024094

Rat/Crl:CD (SD) Oral (gavage) 0, 40, 80, 200

(6 months) 25 M, 25 F ≤ 200 mg/kg: No noteworthy findings.

Cmax values at 40, 80, and 200 mg/kg were up to 2,650; 22,700; and 124,000 μg/mL.

GLP DM08025/

930039270

Rat/Crl: CD (SD) Oral (gavage) BMS-650032:

0, 30, 60 BMS-790052:

0, 10, 60 (1 month)

10 M, 10 F BMS-650032/BMS-790052 at

≤ 60/60 mg/kg: No drug-related CNS, or respiratory effects

BMS-650032: Cmax ≤ 15.2 μg/mL BMS-790052: Cmax ≤ 5.7 μg/mL

GLP DS08126/

930035562

Cardiovascular, Neurologic, and Respiratory

Dog/Beagle Oral (capsule) 0, 20, 60, 300

(1 month) 3 M, 3 F ≤ 300 mg/kg: No noteworthy findings.

Cmax values at 20, 60, and 300 mg/kg were up to 6.12, 28.9, and 114 μg/mL.

GLP DM07020/

930024088

Table 2.6.3.4: Safety Pharmacology

Test Article: Asunaprevir (BMS-650032) Organ Systems

Evaluated Species/

Strain Method of

Administration Doses (mg/kg)

Gender and No.

per Group Noteworthy Findings GLP

Compliance

Study No./

Document Control Cardiovascular, No.

Neurologic, and Respiratory

Dog/Beagle Oral (capsule) 0, 15, 50, 100

(9 months) 4 M, 4 F ≤ 100 mg/kg: No noteworthy findings.

Cmax values at 15, 50, and 100 mg/kg were up to 6.29, 26.8, and 59.7 μg/mL.

GLP DM08026/

930038894

Rat/Crl: CD (SD) Oral (gavage) BMS-650032:

0, 30, 60 BMS-790052:

0, 10, 60 (1 month)

10 M, 10 F BMS-650032/BMS-790052 at

≤ 60/60 mg/kg: No drug-related CNS, or respiratory effects

BMS-650032: Cmax ≤ 15.2 μg/mL BMS-790052: Cmax ≤ 5.7 μg/mL

GLP DS08126/

930035562

Monkey/

Cynomolgus Oral (gavage) BMS-650032:

0, 72, 129.5 BMS-790052:

0, 15, 50 (1 month)

4 M, 4 F BMS-650032/BMS-790052 at

≤ 129.5/50 mg/kg: No drug-related CV, CNS, or respiratory effects.

BMS-650032: Cmax ≤ 18.1 μg/mL BMS-790052: Cmax ≤ 4.65 μg/mL

GLP DS08143/

930035546

Monkey/

Cynomolgus Oral (gavage) BMS-650032:

0, 45, 80 BMS-790052:

0, 15, 50 (3 months)

4 M, 4 F BMS-650032/BMS-790052 at

≤ 80/50 mg/kg: No drug-related CV, CNS, or respiratory effects.

BMS-650032: Cmax ≤ 9.00 μg/mL BMS-790052: Cmax ≤ 3.75 μg/mL

GLP DM09008/

930039780

Abbreviations: Cmax = Mean maximum plasma drug concentration; CNS = Central nervous system; CV = Cardiovascular; HEK = Human embryonic kidney cells; hERG = Human ether-a-go-go-related gene; Hz = Hertz; IV = Intravenous; L-type = Long acting-type; NZW = New Zealand white; PEG = Polyethylene glycol; Peg IFN = Pegylated interferon α-2b;

qod = Every other day; RBV = Ribavirin; SD = Sprague Dawley; TPGS = d-α-tocopheryl polyethylene glycol 1000 succinate.

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