INORGANIC NANOPARTICLE-BASED VACCINE COMPOSITIONS FOR CANCER TREATMENT
20230226163 · 2023-07-20
Inventors
- Gustavo González Ruiz (La Habana, CU)
- David Alejandro González Martínez (La Habana, CU)
- Fernando Bordallo León (La Habana, CU)
- Belinda Sánchez Ramírez (La Habana, CU)
- Kalet León Monzón (La Habana, CU)
- Yerandy Echeverría Luna (La Habana, CU)
- Maria del Carmen Luzardo Lorenzo (La Habana, CU)
- Mabel Cruz Rodríguez (La Habana, CU)
- Adys González Palomo (La Habana, CU)
- Julio Felipe Santo Tomás Pompa (La Habana, CU)
- Judey Aymed García Artalejo (La Habana, CU)
- Elaine Ruiz Castro (La Habana, CU)
- Lien López Matilla (La Habana, CU)
Cpc classification
A61K2039/6037
HUMAN NECESSITIES
A61K2039/55555
HUMAN NECESSITIES
International classification
Abstract
The present invention is related to biotechnology, particularly to the field of human health. It provides new vaccine compositions that comprise as active principle a system that contains the recombinant human EGF, or peptides thereof, and a carrier protein or peptide, bound to a nucleus constituted by inorganic nanoparticles, with nanometric or submicrometric scale dimensions. These vaccine compositions are useful for the chronic treatment of cancer and have as advantages that their administration does not result in the appearance of adverse effects at the injection site and that they do not accumulate in the body.
Claims
1. A vaccine composition to induce an immune response against the epidermal growth factor (EGF), comprising as active principle a system that contains the recombinant human EGF (rhEGF), or peptides thereof, and a carrier protein, bound to a nucleus formed by inorganic nanoparticles.
2. The vaccine composition of claim 1, wherein the inorganic nucleus is formed by salts, oxides or hydroxides selected from the group comprising of: calcium, iron, zinc, magnesium, zirconium, cerium, beryllium, silicon, or the mixture of two or more of them.
3. The vaccine composition of claim 1, wherein the nucleus is of calcium phosphate.
4. The vaccine composition of claim 3, wherein the calcium phosphate is hydroxyapatite (HAp).
5. The vaccine composition of claim 4, wherein the HAp is of amorphous type.
6. The vaccine composition of claim 4, wherein the HAp has low cristallinity.
7. The vaccine composition of claim 4, wherein the hydroxyapatite is partially coated by an organic ligand.
8. The vaccine composition of claim 7, wherein the organic ligand is sodium citrate.
9. The vaccine composition of claim 1, wherein the carrier protein is selected from the group comprising: cholera toxin B subunit, tetanus toxoid, KLH, and P64k of Neisseria meningitidis.
10. The vaccine composition of claim 1, wherein the active principle is on the surface of a HAp nanoparticle.
11. The vaccine composition of claim 10, characterized by wherein the active principle is bound to the HAp nanoparticle by means of one of the following methods: Covalent bond of the chemical conjugate of the rhEGF or peptides thereof and the carrier protein or peptide with the HAp nanoparticle. Covalent bond of the rhEGF or peptides thereof and the carrier protein or peptide with the HAp nanoparticle in an independent way. Successive covalent bond of the rhEGF or peptides thereof and the carrier protein or peptide with the HAp nanoparticle. Multiple conjugation of the rhEGF or peptides thereof and the carrier protein or peptide on the surface of the HAp. Encapsulation or physical binding of the rhEGF and the carrier protein or peptide on the surface of the HAp.
12. The vaccine composition of claim 1 in combination with other adjuvants that are selected from the group consisting of: incomplete Freund's adjuvants, squalene-based adjuvants, synthetic origin adjuvants, mineral origin adjuvants, vegetable origin adjuvants, animal origin adjuvants, particulated proteic adjuvants and liposomes.
13. A method of treating cancer comprising administering the vaccine composition of claim 1.
14. A method of treating a disease for a subject in need thereof comprising administering a therapeutically effective amount of the vaccine composition of claim 1.
15. The method of claim 14, wherein a previous immune response induction stage is achieved with another vaccine composition against the EGF.
Description
BRIEF DESCRIPTION OF THE FIGURES
[0091] FIG. 1. X-Ray Diffraction Pattern: A) Amorphous HAp particles, obtained in the present invention. B) Standard HAp pattern—JCPDS: PDF Ref. 09-0432.
[0092] FIG. 2. FTIR Spectrum: A) Amorphous HAp particles obtained in the present invention. B) Sodium citrate.
[0093] FIG. 3. Size of the amorphous HAp particles obtained in the present invention, determined by electronic transmission microscopy. A) Image of the particles recorded at 25000× magnification. B) Image of the particles recorded at 500000× magnification. C) Size distribution of the particles.
[0094] FIG. 4.Thermogram of the amorphous HAp nanoparticles obtained in the present invention.
[0095] FIG. 5. Size distribution of the HAp-rhEGF-rP64k system covalently bound, determined by the method of dynamic light scattering (DLS).
[0096] FIG. 6. Characterization of the HAp-rhEGF-rP64k system by means of: A) SDS-PAGE: 1—Molecular mass pattern 2—Positive control of the rhEGF-rP64k conjugate elaborated according to U.S. Pat. No. 8,778,879, invention 3—HAp-rhEGF-rP64k system. B) Western Blot profile: 1—Positive control of rhEGF-rP64k conjugate, 2—HAp-rhEGF-rP64k system.
[0097] FIG. 7. Anti-EGF antibody response of the C57BL/6 mice immunized with the HAp-rhEGF-rP64k system covalently linked and the control group (Montanide-rhEGF-rP64k).
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EXAMPLES
Example No. 1. Synthesis, Characterization and Activation of HAp Nanoparticles
[0111] Following a modified variant of the procedure described by Koroleva M., et al., Russian Journal of inorganic chemistry (2016), 61(6): 674-680), nanoparticles of amorphous HAp coated with sodium citrate were obtained. A solution was prepared under controlled environmental conditions, formed by CaCl.sub.2 0.05 mol/L and sodium citrate at a sodium citrate/calcium molar ratio of 4:1 (A solution). Next, a sterile B solution was added, formed by NaH.sub.2PO.sub.4 0.06 mol/L at a flow rate of 1 mL/min, maintaining a Ca/P molar ratio of 1.67. Subsequently, the reaction was adjusted to pH 10 with a dissolution of sodium hydroxide and it was kept stirring for three hours at room temperature. Once the reaction was concluded, it was washed with purified water and separated by filtration using Amicon polyethersulf one membrane of 10 kDa. The obtained solid was vacuum dried at room temperature. Next, they were sterilized with pure steam at 120° C. for 30 min and vacuum dried.
[0112] By means of the X-Rays Diffraction assay it was demonstrated that HAp amorphous nanoparticles, with crystallinity degree of 9.3% and crystallite size of 16.5 nm were generated (
[0113] The Fourier transformed infrared spectra (FTIR) of the nanoparticles (A) and the sodium citrate used as control (B) are shown in
[0114] The nanoparticles, determined by Electronic transmission Microscopy, presented a spherical morphology (
[0115] In the thermography a loss of 6.2% of the mass at temperatures higher than 200° C. (
[0116] The nanoparticles of amorphous HAp were treated with a sterile dissolution of EDC maintaining a mass ratio EDC/HAp of 2:1 for one hour, under controlled environmental conditions. Then the suspension was centrifuged at 6708 gravities and the excess EDC was removed.
Example 2. Obtainment of the HAp-rhEGF-rP64k System by Means of the Covalent Bond Between the Amorphous HAp Nanoparticles and the rhEGF-rP64k Conjugate
[0117] The nanoparticles of amorphous HAp obtained and activated with the procedure described in Example 1 were mixed under controlled environmental conditions, with a sterile solution of PBS, pH 7±0.3, containing the rhEGF-rP64k chemical conjugate obtained with the methodology described in U.S. Pat. No. 8,778,879 invention at a rhEGF-rP64k/HAp mass ratio of 1:2.5. The suspension formed was kept under shaking at 140 cycles per minute for 2 h at room temperature.
[0118] The HAp-rhEGF-rP64k system obtained was dispersed with EDTA, the conditions of the medium were adjusted to a pH of 7±0.3 and protein concentration of 1±0.2 mg/mL, with sterile solutions of PBS and sodium hydroxide.
[0119] The DLS assay showed the presence of nanoparticles with mean hydrodynamic diameter of 97.5 nm and a polydispersity index of 0.36. The obtained system was polydisperse with particle diameter ranging from 9 to 366 nm, measured by intensity (
[0120] The nanoparticulate system, obtained by means of the previously explained procedure, was characterized by means of SDS-PAGE and Western Blot (
Example 3. The HAp-rhEGF-rP64k System Generates a Humoral Response Against the EGF Without Visible Adverse Effects at the Injection Sites.
[0121] C57BL/6 (n=5) mice were immunized with 63 μg of proteins, contained in the system described in Example 2. A batch of the product obtained with the methodology described in U.S. Pat. No. 8,778,879 invention (Montanide-rhEGF-rP64k) was used as positive control of the assay. An immunization protocol consisting of four doses was applied (days: 0, 14, 28 and 42).
[0122] Two days before beginning the immunization protocol and on days 35 and 56, the total IgG antibody titers against the EGF were determined in both groups of mice by means of ELISA. The ratio (IgG2b+IgG2c)/IgG1 specific to the EGF was also determined in the immune sera on day 56. The statistical analysis was performed using the test of comparison of means of Kruskal-Wallis, different letters showed statistically significant differences (p<0.05).
[0123] The HAp-rhEGF-rP64k system generated anti-EGF antibodies, that were detectable in the immune serum at a dilution of 1/10000 on day 56 (
[0124] The effect of the HAp-rhEGF-rP64k system at the injection site was determined. To this, purpose five BALB/c mice were treated with the anti-EGF system described in Example 2 (HaP-rhEGF-rP64k) and five with the Montanide-rhEGF-rP64k control. The vaccination protocol was similar to the one previously described. After concluding the experiment, photographic images of the injection sites of the mice from the two treated groups were taken. As can be seen in
Example 4. The Combination of the HAp-rhEGF-rP64k System with Particulate Adjuvants Generates an Anti-EGF IgG Antibody Response and Induces a Th1-type Response Pattern
[0125] C57BL/6 mice divided into three groups of five animals each were used. The animals were immunized in the following way:
[0126] Group 1: 63 μg of proteins of the vaccine composition described in U.S. Pat. No. 8,778,879 (Montanide-rhEGF-rhP64k) (Positive control).
[0127] Group 2: 63 μg of proteins of the HAp-rhEGF-rP64k system with 100 μg of proteins of the nanoparticulate adjuvant VSSP.
[0128] Group 3: 31.5 μg of proteins of the HAp-rhEGF-rP64k system and 31.5 μg of the rhEGF-rP64k conjugate, encapsulated in liposomal vesicles (DRV's) obtained by the methodology of dehydration-rehydration (Kirby and Gregoriadis, Biotechnology, (1984) 2: 979-984).
[0129] The immunizations were carried out on days 0, 14, 28 and 42. Blood extractions were performed two days before the beginning of the protocol and on days 35 and 56 and the total IgG antibody titers against the EGF in the serum obtained was determined by means of ELISA. The ratio (IgG2b +IgG2c)/IgG1 specific to the EGF in the sera was also determined on day 56. The statistical analysis was performed by means of the test of comparison of means of Kruskal-Wallis, different letters indicate statistically significant differences (p<0.05). The generation of anti-EGF antibodies was evidenced in the three groups studied. The combinations of the HAp-rhEGF-rP64k system with the VSSP and the DRV's liposomes produced antibodies that were detectable in the immune serum up to a dilution of 1/10000 and were same during the two extractions (FIG. 10). The existence of statistically significant differences of the combination with respect to the control was demonstrated.
[0130] The analysis of the ratio (IgG2b+IgG2c)/IgG1 specific to the EGF on day 56, evidenced both adjuvant combinations exhibited similar responses, and they were both statistically superior as compared to the control (
Example 5. The HAp-rhEGF-rP64k System Maintains the Anti-EGF IgG Antibody Response Previously Induced with Montanide-rhEGF-rP64k
[0131] Three groups of C57BU6 mice were used (n=5), which were immunized on days: 0, 14, 28, 42 and 70, with the following immunization schedules:
[0132] Group 1. (Control) the mice were immunized with 63 μg of proteins contained in the system described in U.S. Pat. No. 8,778,879 patent (Montanide-rhEGF-rhP64k).
[0133] Group 2. The mice were immunized on day 0 with 63 μg of proteins contained in the Montanide-rhEGF-rhP64k system and with same quantity of proteins contained in the HAp-rhEGF-rP64k system on the rest of the immunizations performed.
[0134] Group 3. The mice were immunized on days 0 and 14 with 63 μg of proteins contained in the Montanide-rhEGF-rhP64k system and with same quantity of proteins contained in the HAp-rhEGF-rP64k system on the rest of the immunizations performed.
[0135] Two days before to the first immunization, the pre-immune serum was extracted and on days 35, 56 and 84 days the extractions of the immune sera were performed and the total IgG antibody titers against the EGF were quantified by means of ELISA.
[0136] Anti-EGF antibody titers were detectable at the three times studied in the three groups, without statistical significant differences across them, at the 1/50000 dilution on day 35 and at the 1/100000 dilution on days 56 and 84 (
Example 6. Construction of the HAp-PI system by Means of the Covalent Binding of the rhEGF and rP64k Proteins on the Surface of the Amorphous HAp Nanoparticles
[0137] The HAp nanoparticles previously coated with sodium citrate and activated with EDC, obtained according to the methodology described in Example 1, were mixed under controlled environmental conditions with a sterile PBS solution, pH 7±0.3, containing rhEGF and rP64k at a molar ratio of 6 rhEGF per rP64k and proteins/HAp mass ratio of 1: 2.5. The suspension formed was kept under shaking at 140 cycles per minute for 2 h at room temperature. By means of this procedure, a rhEGF-HAp-rP64k system was obtained characterized in that the proteins are bound to the HAp nanoparticle but not to each other. This system was dispersed with EDTA, adjusting the pH to 7±0.3 and the protein concentration to 1±0.2 mg/mL.
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[0139] As can be seen in
[0140] As evidenced in
Example 7. Construction of the HAp-CM System on the Surface of the Amorphous HAp Nanoparticles by Means of the Multiple Conjugation of the rhEGF and rP64k Proteins
[0141] The amorphous HAp nanoparticles obtained in Example 1 were treated under controlled environmental conditions for 1 h with a sterile EDC solution, maintaining a mass ratio of 2.7 EDC per HAp. Next, a sterile PBS solution, pH 7±0.3, was added containing the rhEGF and rP64k at a molar ratio of 6 rhEGF per rP64k and proteins/HAp mass ratio of 1:2.5. The suspension formed was kept under shaking at 140 cycles per minute for 2 h at room temperature.
[0142] A system formed by HAp nanoparticles coated with both recombinant proteins bound to each other and to the nanoparticles was obtained as a result of this procedure. This system was dispersed with EDTA and the pH was adjusted to 7±0.3. Subsequently, it was diluted with PBS solution until a protein concentration of 1±0.2 mg/mL was reached.
[0143] By means of the multiple conjugation previously described, a complex HAp-rhEGF-rP64k system with mean size of 90.2 nm, measured by DLS, and polydispersity index of 0.337 was obtained (
[0144] The characterizations performed by means of the SDS-PAGE electrophoresis and Western Blot showed the conjugation of the proteins. A similar product to the rhEGF-rP64k positive control, that recognizes the anti-EGF antibodies, was obtained (
Example 8. The New Systems Constructed on the HAp Nanoparticles Generate Anti-EGF IgG Antibody Responses and Produce a Smaller Number of Epidermal Lesions at the Injection Site
[0145] Three groups of five C57BL/6 mice each were immunized, with 63 μg of proteins, contained in the following systems:
[0146] Group 1: HAp-rhEGF-rhP64k system, obtained according to the methodology described in Example 2.
[0147] Group 2: HAp-PI system, obtained according to the methodology described in Example 6.
[0148] Group 3: HAp-CM system, obtained according to the methodology described in Example 7.
[0149] The immunizations were performed on days 0, 14, 28 and 42. Blood extractions were carried out two days before the beginning of the protocol and on days 35 and 56. The total IgG antibody titers against the EGF in the obtained sera were determined by means of ELISA. The ratio (IgG2b+IgG2c)/IgG1 specific to the EGF in the sera was also determined on day 56. The statistical analysis was performed by means of the test of comparison of means of Kruskal-Wallis, different letters indicate statistically significant differences (p<0.05).
[0150] The HAp-rhEGF-rP64k and HAp-CM systems generated anti-EGF antibodies that were detectable in the immune serum up to a dilution of 1/10000 and in the HAp-PI system up to a dilution of 1/8000 on days 35 and 56 (
[0151] The analysis of the ratio (IgG2b IgG2c)/IgG1 revealed there were no statistically significant differences in the response produced by them. The prevailing responses were of humoral type (Th2), which makes them appropriate for the depletion of the EGF, as part of the treatment of epithelial tissue origin cancer. (
[0152] At 120 days after the beginning of the experiment, the C57BL/6 mice were sacrificed and tissue samples from the injection sites were extracted for the anatomopathological analysis, previously staining them with hematoxylin-eosin. The tissue sections were fixed in neutral buffered formalin and they were processed by means of the paraffin embedding method. As can be seen in
[0153] In each mouse of the three previous groups, the presence or absence of the following lesions was evaluated:
[0154] Discontinuity of the epidermis and lymphocytic infiltration of the dermis.
[0155] Inflammatory infiltrate.
[0156] Invasion of the muscle tissue.
[0157] Vacuolar degeneration of epithelial cells.
[0158] Dilated blood vessels.
[0159] A point was added whenever a lesion was found, the values corresponding to each mouse in the groups were added up and the result was graphed.
[0160] The study evidenced that the groups treated with the systems developed in the present invention exhibited a very small number of lesions, contrary to that observed in the control group inoculated with the Montanide-rhEGF-rP64k system (
[0161] These results corroborate the low toxicity of the anti-EGF systems based on HAp nanoparticles and the adverse effects in the injection sites caused by the mineral oil contained in the Montanide-rhEGF-rP64k system.