Source: PURDUE UNIVERSITY submitted to NRP
CHARACTERIZATION OF CDC14 FUNCTION AND ITS POTENTIAL AS A DRUG TARGET IN PLANT FUNGAL PATHOGENS
Sponsoring Institution
National Institute of Food and Agriculture
Project Status
COMPLETE
Funding Source
Reporting Frequency
Annual
Accession No.
1003606
Grant No.
(N/A)
Cumulative Award Amt.
(N/A)
Proposal No.
(N/A)
Multistate No.
(N/A)
Project Start Date
Oct 1, 2014
Project End Date
Sep 30, 2019
Grant Year
(N/A)
Program Code
[(N/A)]- (N/A)
Recipient Organization
PURDUE UNIVERSITY
(N/A)
WEST LAFAYETTE,IN 47907
Performing Department
Biochemistry
Non Technical Summary
Fungal plant pathogens are a major annual cause of crop damage and loss throughout the world and consequently pose a serious threat to global food supply and security 18. Despite the use of disease-resistant varieties and fungicide applications, many common fungal pathogens continue to cause widespread damage to important global crop species, including rice (Magnaporthe oryzae), and cereals (Fusarium graminearum)18. Inevitably, pathogens evolve resistance to fungicides and overcome disease-resistant cultivars7. Thus, additional treatment options, including novel anti-fungal targets are constantly needed to limit crop damage from fungal pathogens. In a recent ranking of the top 10 scientifically and economically important fungal plant pathogens by the journal Molecular Plant Pathology, Magnaporthe oryzae and Fusarium graminearum were ranked first and fourth, respectively7.Cdc14 is an attractive target for anti-fungal drug development for several important reasons. First, genetic deletion of CDC14 severely retards growth and eliminates pathogenicity of F. graminearum and M. oryzae, based on results from our Purdue collaborator, Dr. Jin-Rong Xu. Second, unlike most serine/threonine phosphatases, Cdc14 is a single subunit enzyme whose substrate selectivity appears to be entirely dictated by the structure around its catalytic site, suggesting that design of highly specific competitive inhibitors should be achievable. Third, CDC14 phosphatase genes are conserved in fungi and animals, but are absent from higher plants11. Thus, plants are likely to be unaffected by compounds that specifically inhibit Cdc14. The proposed work will address the problem of crop fungal pathogens by understanding the physiological importance of a protein required for plant infection and by developing inhibitors to test the viability of this protein as a novel anti-fungal drug target.The potential outcomes and benefits to society are the future development of new anti-fungal compounds for treating or preventing plant fungal infections that cause devastating losses to crops around the world each year.
Animal Health Component
(N/A)
Research Effort Categories
Basic
100%
Applied
(N/A)
Developmental
(N/A)
Classification

Knowledge Area (KA)Subject of Investigation (SOI)Field of Science (FOS)Percent
2124020100075%
2124020103025%
Goals / Objectives
1. Characterize the enzymatic specificity of Fusarium graminearum and Magnaporthe oryzae Cdc14 phosphatases (FgCdc14 and MoCdc14).2. Use combined bioinformatic (from Objective 1) and biochemical approaches to identify physiological substrates of FgCdc14 and MoCdc14.3. Characterize the phenotypes associated with perturbed phospho-regulation of select substrates from Objective 2.4. Develop specific inhibitors of Cdc14 phosphatases using high throughput screening5. Test effectiveness of Cdc14 inhibitors identified and developed in Objective 4 towards F. graminearum and M. oryzae in vivo and in plant infection assays.
Project Methods
Objective 1. FgCdc14 and MoCdc14 will be characterized to determine if the same determinants of substrate recognition identified in budding yeast and human Cdc14 enzymes exist in these fungal orthologs.Positional scanning phosphopeptide libraries will define the substrate features that promote or inhibit efficient Cdc14 activity. We have executed this approach withSaccharomyces cerevisiaeCdc14 (ScCdc14) but intend to fully characterize the contributions of amino acids at several positions before and after pSer-Pro, which is the essential core sequence of Cdc14 substrates4. We will test all possible amino acids at positions -2, -1, +2, +4, +5, and +6 relative to pSer because these residues are predicted to contact the highly conserved substrate binding channel on Cdc14. Three libraries will be synthesized. All will have pSer-Pro fixed at the 0 and +1 positions. One will have a fixed +3 Lys (optimal), one a fixed +3 Arg (less optimal), and one will leave +3 unfixed. FgCdc14 and MoCdc14 will be compared to ScCdc14. This broader analysis of phosphopeptide substrates has the potential to reveal additional positive and negative determinants of substrate selection and will allow more refined prediction using bioinformatic tools (Objective 2).Screening phosphopeptide libraries is simple8. Purified recombinant Cdc14 is mixed with a fixed low concentration (below Km) of purified synthetic phosphopeptide substrates in 384 well plates and incubated 30 min at 30 °C. A commercially available phosphate detection reagent is added, which stops the reaction and forms a green color when complexed with free phosphate. The absorbance is measured at 620 nm in a plate reader. The rate values are approximations of the catalytic efficiency kcat/Km and provide a useful means to compare the relative ability of collections of substrates to be recognized and dephosphorylated by Cdc14.With Dr. Sergey Savinov, Purdue Center for Cancer Research, we will perform docking and molecular dynamics simulations to model the interactions of optimal substrate sequences identified in the peptide library screen with the substrate binding site, based on the existing crystal structure of human Cdc14B10. We will create a homology model of theF. graminearumandM. oryzaeenzymes using the program Prime (Schrödinger, LLC).Objective 2. Using the initial specificity features identified in ScCdc14 we have demonstrated the ability to accurately predict physiological Cdc14 substrates6,9. This approach will be used to predict substrates inF. graminearumandM. oryzae.In parallel with bioinformatics, we will employ biochemical approaches to identify targets of Cdc14 in these two fungal pathogens. One approach relies on use of a substrate trapping mutant of Cdc14 (Cys to Ser mutation in the active site). This mutation eliminates catalytic activity but allows high affinity substrate binding. It has been used previously in proteomic workflows to globally identify Cdc14 interaction partners and substrates in common model organisms2,5. We have generated the substrate trap mutation in theCDC14genes ofF. graminearumandM. oryzaefor expression and purification of the mutant proteins as GST fusions in E. coli. The mutant fusion proteins will be bound to glutathione agarose to create an affinity column and soluble whole cell extracts ofF. graminearumandM. oryzaecultures will be passed through the column. After extensive washing, proteins will be eluted and subjected to HPLC-coupled tandem mass spectrometry (MS) in the Purdue Proteomics Facility. Dr. Xu will introduce epitope tagged substrate trap alleles into the genomes ofF. graminearumandM. oryzae. The tagged FgCdc14 and MoCdc14 proteins will be affinity-purified from whole cell extracts using commercially available affinity resin and specifically bound proteins identified by MS. Extracts from cells lacking the tagged alleles will serve as a negative control. The list of interaction partners will be filtered using the bioinformatics predictions to find the most promising candidate substrates.To validate top candidates, a series of biochemical and biological experiments will be performed6,9. Synthetic phosphopeptides representing the putative Cdc14 target sites will be analyzed in steady-state kinetic assays with recombinant Cdc14 enzymes and compared to our gold standard set of known substrate peptides from budding yeast. Recombinant substrate proteins will be phosphorylated in vitro with purified Cdk1 from budding yeast and subjected to Cdc14 phosphatase assays in which each individual site can be quantitatively monitored by MS8. The candidate substrate sites will be compared to known high efficiency budding yeast Cdc14 substrates. With Dr. Xu, we will monitor the phosphorylation status of tagged alleles of the candidate substrates in vivo in wild-type andcdc14null strains ofF. graminearumandM. oryzaeusing Phos-tag SDS-PAGE gels and immunoblotting. We expect phosphorylated forms of the substrates to be enhanced in the absence of Cdc14 function. We will introduce additional copies of Cdc14 for overexpression and evaluate phosphorylation status on Phos-tag SDS-PAGE by immublotting. We expect phosphorylation to be reduced upon Cdc14 overexpression. Interaction between the candidate substrate and Cdc14 should be dependent on Cdk phosphorylation sites. We will introduce mutant alleles of the candidate substrates lacking Cdk sites and perform co-IP analysis with the substrate trap variants of Cdc14 to determine if recognition is direct and dependent on Cdk phosphorylation.Objective 3. We will select validated Cdc14 substrates from Objective 2 inF. graminearumfor initial functional characterization of phosphoregulation. The Xu lab will perform genetic replacement of wild-type alleles of the substrate candidates with phosphosite mutants (Ser to Ala to mimic lack of phosphorylation and Ser to Asp to mimic constitutive phosphorylation) to look for phenotypes. Growth rates and plant infectivity will be important for the overall goal of this project, but more specific cell division phenotypes, including DNA damage sensitivity, chromosome mis-segregation, and cytokinesis defects will be of biological interest6,9.Objective 4. We have initiated screening of a diverse small molecule library for Cdc14 inhibitors at the Bindley Bioscience Center. With Dr. Larisa Avrimova we have identified a half dozen lead inhibitors of ScCdc14 thus far (> 75% inhibition using an optimal phosphopeptide substrate and 40 μM each compound), after screening close to 10,000 of the 180,000 compounds at Purdue. We will compare inhibition towards budding yeast Cdc14, FgCdc14, and MoCdc14. We are looking for competitive inhibitors that are highly specific for the Cdc14 family but broadly reactive across fungal species. This will be tested using our standard phosphatase assay and specificity will be assessed using a panel of purified protein phosphatases representing major evolutionary families.The best hits that meet our criteria for specificity and potency will be modeled into the Cdc14 active site by Dr. Savinov. Synthesis of new derivatives of these base compounds will be developed that contribute to substrate recognition. The initial compounds will likely be broadly specific towards many members of the protein tyrosine phosphatase superfamily (of which Cdc14 is member). We expect to generate high affinity specific inhibitors of the Cdc14 sub-family. Rational design and synthesis of derivatives of the base compounds will be conducted with Dr. Antonella Pepe and Dr. Savinov.Objective 5. Practically useful inhibitory compounds must be both bioavailable and bioactive. The most promising inhibitory compounds from objective 4 will be testedin vivoand in plant infection assays to determine if they exhibit these properties. Dr. Xu has expertise in assessing growth rates and phenotypes ofF. graminearumandM. oryzaeand the ability of these species to infect plants.

Progress 10/01/14 to 09/30/19

Outputs
Target Audience:The students performing research in my lab, students in my summer research program related to this project, and students in my lab course at Purdue that is based on this project. Scientists at sites in which I presented the work through talks or posters. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?Graduate student and undergraduate student independent research training High school student training in the summer research program I direct focused on this project Undergraduate teaching in lab course I developed based on this project. How have the results been disseminated to communities of interest?Peer-reviewed research publications Oral presentations at scientific meetingsand invited seminars What do you plan to do during the next reporting period to accomplish the goals? Nothing Reported

Impacts
What was accomplished under these goals? Recruited 2 new graduate students to lab to pick up the projects Developed new assays to look at Cdc14 specificity in diverse plant pathogens under goal 1. Assessed inhibitory effect of a peptide substrate mimic inhibitor against diverse pathogen Cdc14 enzymes under goal 4.

Publications


    Progress 10/01/17 to 09/30/18

    Outputs
    Target Audience:Undergraduate research students in the biological sciences and biochemistry programs. High school students participating in the new Summer Science Program curriculum I developed based on this project. Graduate students in the biochemistry Ph.D. program. The scientific communities that study or are interested in phosphatases, cell division, and fungal pathogens. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?I have 3 newundergrad research students workingon this project and 2 additional students graduate this past year. I have had 2 rotating first yeargraduate students work on the project and hope to recruit one of them to the lab to continue this work. The Summer Science Program curriculum trains talented high school students from around the countryand world in how to conduct biochemistry research. How have the results been disseminated to communities of interest?Summer Science Program results are deposited in the Purdue Research Repository, which is a publicly accessible database for Purdue research projects. No other publications were obtained during this reporting period. What do you plan to do during the next reporting period to accomplish the goals?The main focus will be on obtaining funding so that additional graduate students and/or post-doctoral researchers can be recruited to the project. Undergraduate researchers will continue to work in my lab on the project goals.

    Impacts
    What was accomplished under these goals? Under goal 1 we continue to define mechanisms of substrate selectivity of the Cdc14 family using orthologs from a variety of fungal species. This ties in with projects conducted in the Summer Science Program by high school students. We have identified some new small molecule Cdc14 inhibitors as well as begun efforts to explore peptide-based substrate mimic inhibitors. We continue to characterize mechanisms of inhibiition of these and previouly identified inhibitors. Our structural biology efforts to visualize how Cdc14 enzymes interact with substrates and are inhibited by small molecules identified in our screens are progressing nicely. We have identified conditions to grow Cdc14 crystals, have collected diffraction data and are currently trying to solve structures Cdc14 bound to substrates and inhibitors. In vivo work in the plant pathogen species remains on hold until additional funding is obtained and personnel can be recruited to perform the work.

    Publications


      Progress 10/01/16 to 09/30/17

      Outputs
      Target Audience:Undergraduate research students in the biological sciences and biochemistry programs. High school students participating in the new Summer Science Program curriculum I developed based on this project. Graduate students in the biochemistry Ph.D. program. The scientific communities that study or are interested in phosphatases, cell division, and fungal pathogens. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?I have had 2 undergrad research studentswork on this project this past year. I have had 1graduate studentwork on the project, and publish a paper in Journal of Cell Science on Cdc14 function and mechanism in budding yeast. The Summer Science Program curriculum trains talented high school students from around the countryand world in how to conduct biochemistry research. How have the results been disseminated to communities of interest?During this reporting period primarily through our publication in Journal of Cell Science as well as releaseof data from the Summer Science Program in the Purdue Research Repository, which is a publicly accessible database for Purdue research projects. What do you plan to do during the next reporting period to accomplish the goals?The main focus will be on obtaining funding so that additional graduate students and/or post-doctoral researchers can be recruited to the project. Undergraduate researchers will continue to work in my lab on the project goals.

      Impacts
      What was accomplished under these goals? Under goal 1 we continue to define mechanisms of substrate selectivity of the Cdc14 family using orthologs from a variety of fungal species. This ties in with projects conducted in the Summer Science Program by high school students. We are just beginning to launch new efforts to identify small molecule inhibitors of Cdc14 activity using high throughput screens at the Purdue drug discovery facility. We continue to characterize mechanisms of inhibiition of previouly identified inhibitors. We have inititated structural biology efforts to visualize how Cdc14 enzymes interact with substrates and are inhibited by small molecules identified in our screens. In vivo work in the plant pathogen species remains on hold until additional funding is obtained and personnel can be recruited to perform the work.

      Publications

      • Type: Journal Articles Status: Published Year Published: 2017 Citation: Powers BL, and Hall, MC. Re-evaluating the role of Cdc14 phosphatase in reversal of Cdk phosphorylation during mitotic exit. J Cell Sci. 130: 2673-2681. PMID: 28663385


      Progress 10/01/15 to 09/30/16

      Outputs
      Target Audience:Undergraduate research students in the biological sciences and biochemistry programs High school students participating in the new Summer Science Program curriculum I developed based on this project Graduate students in the biochemistry Ph.D. program The scientific communitiesthat study or are interested inphosphatases, cell division, and fungal pathogens Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?I have had 3 undergrad research students join the lab in the past year and work on this project, including one that participated in Purdue summer undergraduate research program. I have had 2 graduate students work on the project, both of whom have now successfully defended their thesis work and graduated. The Summer Science Program curriculum trains talented high school students from around the countryand world in how to conduct biochemistry research. How have the results been disseminated to communities of interest?Presentations at meetings by my graduate students, including the U.S. HUPO annual meeting, and the Cold Spring Harbor Cell Cycle meeting. What do you plan to do during the next reporting period to accomplish the goals?The main focus will be on obtaining funding so that additional graduate students and/or post-doctoral researchers can be recruited to the project. Undergraduate researchers will continue to work in my lab on the project goals.

      Impacts
      What was accomplished under these goals? Under goal 4 we have continued to characterize the mechanisms of action of many of the lead compounds that came out of our high throughput screening for Cdc14 phosphatase inhibitors and to understand the specificity of these inhibitors, both against Cdc14 orthologs from diverse fungal species, and against other unrelated phosphatases. Under goal 1 we have continued expanding our biochemical characterization of Cdc14 orthologs from additional plant pathogen species through overexpression and purification from E. coli and enzymatic assays to define substrate specificity. This is largely through the new Summer Science Program curriculum where high school students characterize novel Cdc14 enzymes. No additional progress has been made on goals 2, 3, and 5 due to absence of funding and personnel

      Publications


        Progress 10/01/14 to 09/30/15

        Outputs
        Target Audience:The target audience was the scientific research community interested in plant fungal pathogens, mechanisms of plant infection by pathogens, and development of anti-fungal agents to combat plant infection. Changes/Problems: Nothing Reported What opportunities for training and professional development has the project provided?I have one graduate student assigned to this project. He was an author on our Molecular Microbiology paper on FgCdc14. He has conducted all of the high throughput screening for inhibitors and performed all the biochemical characterization of fungal Cdc14 enzymes. His training in enzymology and various aspects of drug discovery has been a major focus. He will be graduating with his Ph.D. this year. I hope to attract another graduate student to the project and a couple undergraduates from our program this year. I use the topic of this research project as the basis for the Analytical Biochemistry lab course that I teach at Purdue. I educate around 18 students each fall semester in this course on modern biochemistry lab techniques as applied to purification and characterization of an enzyme (in this case Cdc14 - we are currently using the enzyme from Ustilago maydis) I have developed a summer research curriculum for high school students as part of the expansion of the Summer Science Program. The high school students will be purifying Cdc14 enzymes from plant fungal pathogens, characterizing their enzymatic properties and exploring the development of inhibitors for these enzymes using biochemical and computational tools. Two undergraduate students tested proof of principle this past summer. We will have a full test of the program this coming summer with a small number of students before it is fully implemented in the summer of 2017. How have the results been disseminated to communities of interest?We have published two papers this past year, one a research article on characterization of Cdc14 in Fusarium graminearum and the other a methods paper on how to characterize the specificity of protein phosphatases using Cdc14 as an example. What do you plan to do during the next reporting period to accomplish the goals?We will continue pushing the research, focusing on the aims above that are not completed yet. I will try to recruit a new graduate student to the project this year, althought it depends on getting funding for the project. I will also attempt to recruit a couple undergraduate students from our program to begin working on the project as well. Much of the work will be performed in our collaborator's lab as well. We have applied for internal funding at Purdue to support the project. We are formulating plans to seek external funding for the project from the NSF and NIFA.

        Impacts
        What was accomplished under these goals? 1. We published a paper this past year with our collaborator from Purdue, Dr. Jin-Rong Xu describing the phenotypes of the plant pathogen F. graminearum when it lacks the CDC14 phosphatase gene. The major finding was that strains lacking Cdc14 are non-infectious, validating Cdc14 as a potential anti-fungal target. Our part of the project was to characterize the enzymatic specificity of purified FgCdc14 enzyme, which we successfully accomplished, and to predict its physiological substrates. Our collaborative team also completed a similar characterization of M. oryzae CDC14 but this has not been published yet. The findings with M. oryzae were similar to F. graminearum. 2. See above in item 1. We completed substrate predictions for FgCdc14 and MoCdc14 and have also gone on to predict substrates from a couple other fungal plant pathogens. We have not yet started on the direct biochemical detection of substrates in these organisms. 3. Goal 3 has not begun yet. 4. We have completed screening of 50,000 compounds from 2 small molecule libraries for inhibitors of the budding yeast Cdc14 enzyme. We have a list of roughly 100 lead candidates that will be subject to validation procedures for reproducibility, effects on Cdc14 from fungal pathogens, mechanim, and specificity for this phosphatase family. We consider the high throughput screening completed now and will be focusing on characterization of the lead componuds we have. 5. We have not begun on this goal yet because we need to narrow our lead list based on mechanism, specificity, potency, and other factors first.

        Publications

        • Type: Journal Articles Status: Published Year Published: 2015 Citation: Powers BL, Melesse M, Eissler CL, Charbonneau H, and Hall MC* (2015). Measuring activity and specificity of protein phosphatases. Methods Mol Biol 1342:221-35. PMID: 26254927 Li C, Melesse M, Zhang S, Hao C, Wang C, Zhang H, Hall MC*, Xu JR* (2015). FgCDC14 regulates cytokinesis, morphogenesis, and pathogenesis in Fusarium graminearum. Mol Microbiol in press. PMID: 26256689