Molecular characterization of zona pellucida glycoproteins: role in fertilization and regulation of fertility


 

Principal Investigator :    Satish K Gupta

Project Associates/ Assistants
Neelu Srivastava
Sangeeta Choudhury
Puja Ramdas (since Aug 2001)
Deepika Batra
Abhishek Upadhyay

PhD Students
Chhabi K Govind (till Jun 2001)
Neela Sivapurapu
Archana Rath
Gagandeep Kaur Gahlay
Sanchita Chakravarty

Collaborators
K Koyama, Hyogo Med College, Japan
C E Rupprecht, CD CP, Atlanta, USA
S V Kapre, Serum Inst of India Ltd, Pune
S S Thakral, CMVL, Meerut Cantt

Major themes of this project are A) Molecular and biochemical characterization of zona pellucida (ZP) glycoproteins and delineation of their role during fertilization, and B) Evaluation of the immunocontraceptive potential of ZP based immunogens. The objectives of the study are (i) expression of non-human primate and canine ZP glycoproteins in various expression systems, (ii) binding characteristics of purified recombinant ZP proteins to spermatozoa in a non-human primate model, (iii) design non-human primate ZP glycoproteins based synthetic peptides and evaluate their immunogenicity, (iv) evaluate immunocontraceptive potential of non-human primate and canine recombinant ZP proteins for fertility regulation in respective homologous animal models and (v) characterization of the immune response to plasmid DNA encoding ZP glycoproteins and rabies glycoprotein-G.

Cloning and expression of non-human primate and canine zona pellucida proteins in baculovirus expression system

To express the glycosylated form of r-bmZP2, the full length cDNA (1.8 kb), excluding the N-terminal signal sequence and C-terminal transmembrane-like domain was PCR amplified and cloned downstream of a late polyhedrin promoter in BioBlueTM-His6 baculovirus transfer vector under EcoR I-Bgl II restriction sites. The plasmid DNA (BioBlueTM-bmZP2) was co-transfected with BaculoGoldTM baculovirus DNA in Sf9 cells and a positive plaque was picked up for further studies. The recombinant protein was expressed as a fusion protein with blue fluorescence protein (BFP) and His6 tag. Time course experiments showed that the maximum expression of the protein occurred 72 hr post infection. The recombinant protein was purified by Ni-NTA column in the presence of urea, which was dialyzed out in renaturing buffer. It showed an apparent molecular weight of 100 kDa in western blot.

Similarly, recombinant dog ZP2 (r-dZP2) and dog ZP3 (r-dZP3) glycoproteins were also expressed as BFP-His6 fusion proteins in Sf9 cells. The expressed proteins showed a band corresponding to 100 and 66 kDa respectively in western blot. Attempts are being made to purify r-dZP2/r-dZP3 and to optimize conditions for cleavage of the BFP-His6 tag from the expressed r-dZP2/r-dZP3.

Structural elucidation of r-bmZP3

As reported last year, we were able to purify the E. coli expressed r-bmZP3 in the absence of chaotropic agents. Further to that, it was subjected to the following circular dichroism (CD) spectroscopic studies to evaluate its secondary structural attributes. All the CD spectra were recorded using a 0.1 cm path length cuvette in 20 mM Tris buffer, pH 8.5 in a spectral range from 195-260 nm. The r-bmZP3 showed a shift in the spectral minima, when the concentration was lowered from 25 mM to 12.5 mM. At 50 and 25 mM concentrations, the protein showed a minima around 225 nm, which shifted to 212 nm at 12.5 mM concentration and remained unchanged till 3 mM. At 12.5 mM concentration, the protein showed a predominantly b sheet structure, though a reasonable a helical component was also observed.

In order to further investigate the structure-activity relationship of bmZP3 protein, computer aided similarity searches across various species were performed. As a result, a core fragment of the
r-bmZP3 starting from the 39 –307 amino acids (aa) was identified. This fragment r-bmZP3
(39-307 aa) was cloned in the pQE30 vector, in-frame downstream of the T5 promoter, between the BamHI and SacI restrictions sites. The protein was expressed in the SG13009[pRep4] strain of E. coli and purified in solubilized form. The r-bmZP3(39-307 aa) showed spectral minima at 223.4 nm at 50 mM concentration which shifted to 215.4 nm at 25 mM and did not show a considerable change up to 3mM, beyond which the concentration effect was not studied due to poor signal to noise ratio. At 12.5 mM concentration, the protein, like its full-length version, had a predominantly b sheet structure with an a helical component. The protein was found to maintain a reasonably stable secondary structure profile over a pH range from 4.5 –8.5. The protein appeared to loose a major portion of the a helical component at highly acidic pH (2.5), though the b sheet remained largely unaffected. The variable temperature study conducted over a wide range of temperature (4°C-90°C) revealed no significant loss of any of the secondary structure component up to 70°C. However, at 90°C the protein lost almost all the b sheet component, though the a helix remained unaffected. This loss of secondary structure was found to be reversible as the b sheet structure was regained after the same sample was incubated at room temperature for a period of 1 hr and re-subjected to CD spectroscopy.

Cloning and expression of recombinant rabies virus glycoprotein-G (r-rG) in E. coli and baculovirus expression system

In order to clone rabies virus glycoprotein G (rG), BHK21 cells were infected with PM10 strain of rabies virus. Total RNA from the infected cells was prepared at various time periods post – infection using TRIZOL reagent. Total RNA was directly used to amplify the cDNA corresponding to r-rG without signal sequence and transmembrane like domain by RT-PCR which resulted in the amplification of a 1.313 kb fragment. Comparison of the nucleotide sequence of the cloned rG with sequences from Gene Bank revealed an identity with other strains ranging from 86-99.9%. The deduced amino acid sequence revealed 100% identity with the sequence having an Accession No. M81058. The 1.313 kb fragment was excised with Bam H I and Kpn I restriction enzymes from PCR-Script SK (+)-rG clone, purified and cloned in-frame downstream of His6 tag under T5 promoter – lac operator control in pQE30 expression vector. Positive clones were identified and checked for expression of r-rG by SDS-PAGE and immunoblotting using a commercially available human rabies immunoglobulin. The western blot analysis revealed a band of approximately 55 kDa. The r-rG protein was purified under denaturing conditions by Ni-NTA affinity chromatography and antibodies were generated against the recombinant protein in male New Zealand white rabbit.

In order to obtain r-rG in glycosylated form, it was expressed in baculovirus expression system. The pQE-rG plasmid was used as a template to PCR amplify cDNA corresponding to rG with a forward primer incorporating BamH I site and the reverse primer incorporating EcoR I site. The BamH I-EcoR I restricted fragment was cloned into pAcSecG2T vector under the late polyhedrin promoter. The r-rG was expressed as a GST fusion protein wherein the native signal sequence was replaced with the insect signal sequence (gp67) in Sf9 cells. The r-rG showed a band with an apparent molecular weight of 75 kDa in western blot. Attempts are underway to purify r-rG using the glutathione agarose beads and to optimize the conditions for thrombin cleavage.

Immunogenicity of ZP glycoproteins based synthetic peptides

The synthetic peptide immunogens capable of generating antibodies that reacted with native ZP and inhibited sperm-egg interaction corresponding to bmZP1 were reported last year. In addition, 5 synthetic peptides corresponding to bmZP2 (bmZP2(88-102 aa), bmZP2(103-125 aa), bmZP2(124-143 aa), bmZP2(395-407 aa) and bmZP2(532-549 aa)) were made and conjugated individually to DT at a 10:1 molar ratio. Further, two synthetic peptides corresponding to human (h) ZP2 (hZP2(85-109 aa); has 5 changes in aa as compared to bmZP2 sequence and hZP2(103-125 aa); having 3 changes in aa as compared to bmZP2 sequence) were also conjugated to DT. Female BALB/cJ mice were immunized with the individual peptide-DT conjugates. The antisera against bmZP2(124-143 aa), bmZP2(395-407 aa) and bmZP2(532-549 aa) have been analyzed for their recognition of the respective peptide and E. coli expressed r-bmZP2 in an ELISA. Anti-peptide antibodies were generated against the respective peptides but only anti-bmZP2(532-549 aa) recognized r-bmZP2 in an ELISA and also recognized native bonnet monkey zona. The antibodies against hZP2(103-125 aa) evaluated so far, recognized human ZP and also inhibited sperm-egg interaction.

A chimeric protein bmZP13 encompassing bmZP1(246-278 aa) (comprising the aa stretch 248-273, antisera against which inhibited human sperm-egg binding) and bmZP3(324-347 aa) (immunization with this peptide in a homologous model showed block in fertility without concomitant ovarian pathology) was made at the cDNA level, with a tri-glycine spacer separating the individual epitopes. The bmZP13 cDNA was cloned in frame of the polyhistidine tag, downstream of the T5 promoter in pQE30 expression vector. The purification of r-bmZP13 is in progress.

Previously, we have reported expression of the chimeric recombinant protein (r-bmZP123) encompassing the B cell epitopes of bmZP1(132-147 aa), bmZP2(86-113 aa) and bmZP3 (324-347 aa) in E. coli. Analysis of the rabbit polyclonal antibodies generated against r-bmZP123 revealed variable reactivity with the native ZP and also in vitro contraceptive efficacy. The r-bmZP123 has 4 cysteine residues, which may lead to different inter and intra-molecular disulphide bond formations that may influence the antibody response. In order to circumvent this, r-bmZP123 was reduced and the cysteine residues were chemically blocked with iodoacetamide. The reduced and iodoacetamidated r-bmZP123 was conjugated to DT using the ‘two step’ glutaraldehyde method. Two female rabbits (R-67, R-68) were immunized with r-bmZP123-DT conjugate. Antibodies were generated against r-bmZP123, r-bmZP1, r-bmZP2 and r-bmZP3 as determined by ELISA. The sera from both the female rabbits showed reactivity with the whole native bonnet monkey ZP.

Characterization of the immune response to plasmid DNA encoding ZP glycoproteins and rabies glycoprotein-G

Last year, we had reported cloning of bmZP1 cDNA in VR1020 mammalian expression vector (VRbmZP1). Expression of bmZP1 in COS-1 cells was confirmed by flow cytometric analysis and western blot analysis which revealed a protein band of approximately 57 kDa as compared to the calculated molecular weight of 51.4 kDa (including TPA signal sequence), suggesting that ZP1 may be expressed in a glycosylated form. The immunogenicity of VRbmZP1 was evaluated by immunizing male BALB/cJ mice intramuscularly (i.m.) with 100 µg DNA/mouse in saline administered thrice on days 0, 21 and 35. Mice immunized with VRbmZP1 plasmid DNA showed significantly higher anti-r-bmZP1 antibodies in comparison to vector immunized mice as determined in an ELISA employing r-bmZP1 expressed in E. coli. The anti-bmZP1 antibodies generated were specific to zona as evident by positive immunofluorescence of VRbmZP1 immunized mice sera with bonnet monkey ovarian sections in an indirect immunofluorescence assay. Also these antibodies inhibited the binding of human spermatozoa to the antibody treated human zona in a hemizona assay thus indicating their immunocontraceptive potential.

After achieving some success with the bmZP1 model, the cDNA corresponding to dZP3, excluding the N-terminal signal sequence and C-terminus transmembrane-like domain, was also cloned in VR1020 (VRdZP3). The immunogenicity of VRdZP3 was analyzed by three different modes of plasmid DNA delivery in male BALB/cJ mice- a) intramuscular (i.m.) administration of DNA in saline, b) i.m. administration of DNA in saline followed by electroporation wherein short electric pulses were given at the site of injection, and c) intradermal administration of DNA entrapped in gold microcarriers and delivered by gene gun. A good antibody response was observed by all the three modes of immunization as determined in an ELISA employing r-dZP3 expressed in E. coli. The anti-dZP3 antibodies also recognized native ZP in an indirect immunofluorescence assay. Interestingly, female BALB/cJ mice immunized with VRdZP3 plasmid DNA by gene gun method, generated antibody response similar to the male mice. These are interesting observations of generating antibodies against ZP3 without coupling to a carrier. The status of fertility of VRdZP3 immunized female mice is under observation.

In the last year report, it was also proposed to make a hybrid construct of dZP3 with rabies glycoprotein-G (rG) with the aim of generating immune response against ZP3 that may block fertility and rG that may provide protection against rabies. Before initiating the making of plasmid DNA construct encoding dZP3-rG hybrid construct, it was pertinent to study immune response to a plasmid DNA encoding rG alone. Two constructs were made using VR1020 vector- (i) rG cDNA excluding the native signal sequence and the transmembrane- like domain (rGVR), (ii) rG cDNA excluding the native signal sequence and retaining the transmembrane- like domain (rGVRt). Localization studies revealed that the expression of rG with both the constructs was cytosolic. The presence of the transmembrane domain in rG, expressed by rGVRt plasmid DNA, did not lead to anchoring of the protein on the cell membrane. However, rGVRt plasmid DNA elicited higher antibody response as compared to rGVR plasmid DNA, thereby suggesting that the transmembrane- like domain may enhance humoral response against r-rG. The influence of native signal sequence on protein trafficking is being evaluated.

Publications

Original peer-reviewed articles

1.     Srivastava N, Santhanam R, Sheela P, Mukund S, Thakral SS, Malik BS and Gupta SK (2002) Evaluation of the immunocontraceptive potential of Escherichia coli expressed recombinant dog ZP2 and ZP3 in homologous animal model. Reproduction (in press).

2.     Rath A, Choudhury S, Hasegawa A, Koyama K and Gupta SK (2002) Antibodies generated in response to plsmid DNA encoding zona pellucida glycoprotein-B inhibit in vitro human sperm-egg binding. Mol Rep Dev (in press).

3.     Koyama K, Hasegawa A and Gupta SK (2002) Prospect for immunocontraception using the NH2-terminal recombinant peptide of human zona pellucida protein-A (hZPA). Am J Reprod Immunol (in press).

4.    *Gahlay GK, Srivastava N, Govind CK and Gupta SK (2002) Primate recombinant zona pellucida proteins expressed in Escherichia coli binds to spermatozoa. J Reprod Immunol 53:67-77 (*in press last year, since published).

5.     *Kaul R, Sivapurapu N, Afzalpurkar A, Srikant V, Govind CK and Gupta SK (2001) Immunocontraceptive potential of recombinant bonnet monkey (Macaca radiata) zona pellucida glycoprotein-C expressed in Escherichia coli and its corresponding synthetic peptide. Reproductive BioMedicine Online 2:33-39 (*in press last year, since published).

6.     Sivapurapu N, Upadhyay A, Hasegawa A, Koyama K and Gupta SK (2002) Native zona pellucida reactivity and in vitro effect on human sperm-egg binding with antisera against bonnet monkey ZP1 and ZP3 synthetic peptides. J Reprod Immunol (in press).

Reviews/Proceedings

1.    Upadhyay A, Sivapurapu N, Rath A and Gupta SK (2001) Rationale of synthetic peptides as immunogens for vaccine development. Proc Indian Natl Sci Acad B (in press).

Patents

1.    Gupta SK, Kalsi G, Shamim M, Nataraju B and Datta RK. A process for preparing diagnostic monoclonal antibody based system for the rapid detection of nuclear polyhedrosis in Bombyx mori l. Indian patent No. 186538 granted in Sep 2001.

2.    Gupta SK, Shamim M, Ghosh D, Baig M, Nataraju B and Datta RK. A process for producing monoclonal antibodies coated latex beads for the detection of pebrine infection in Bombyx mori l. Indian patent No. 186722 granted in Oct 2001.

3.    Gupta SK, Sharma M, Behera AK, Bisht R and Kaul R. A method of inducing infertility in a mammal, a recombinant protein for inducing such infertility and a process for producing the recombinant protein. Indian patent No. 186770 granted in Nov 2001.