Method Article

Fabricating Tunable Polyacrylamide Hydrogels To Study Matrix Stiffness Effects On Stem Leydig Cells

DOI:

10.3791/71387

June 5th, 2026

* These authors contributed equally

In This Article

Summary

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This protocol describes the fabrication of polyacrylamide hydrogels with tunable stiffness to study the effects of matrix mechanics on stem Leydig cell behavior in a controlled two-dimensional culture system.

Abstract

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Extracellular matrix (ECM) stiffness critically regulates stem cell behavior. Previously, we demonstrated that pathological increases in matrix stiffness during aging disrupt stem Leydig cell (SLC) homeostasis, leading to a decline in testosterone. Building on this discovery, we here present a detailed protocol—originally developed in our laboratory—for fabricating polyacrylamide (PA) hydrogels with tunable stiffness to model the testicular microenvironment in vitro. This method enables reproducible casting of gels across a stiffness range of 1–100 kPa, covering physiological to pathological conditions. Key steps include precise mixing of acrylamide/bis-acrylamide, gel swelling equilibration, surface activation with Sulfo-SANPAH, and collagen coating to support SLC adhesion and culture. We provide optimized formulations for target stiffnesses and troubleshooting guidance for common issues such as incomplete polymerization and poor cell attachment. This system allows systematic investigation of how substrate stiffness modulates SLC proliferation, differentiation, and steroidogenic function under defined 2D conditions. Beyond reproductive biology, it also serves as a valuable platform for mechanobiological studies in other cell types and for screening therapeutics targeting stiffness-related dysfunction.

Introduction

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The mechanical properties of the extracellular matrix (ECM) play a pivotal role in regulating stem cell fate, including proliferation, differentiation, and functional maintenance1,2,3,4. In the testis, age-related ECM stiffening has been implicated in the decline of testosterone production. However, the underlying mechanobiological mechanisms remain poorly understood, partly due to a lack of standardized in vitro models that faithfully recapitulate the physiological stiffness range of the testicular niche. The physiological stiffness of young mouse testicular tissue is approximately 1–15 kPa, whereas aged or fibrotic tissue can reach 20–30 kPa or higher.

Polyacrylamide (PA) hydrogels have emerged as a versatile platform for studying cell–matrix interactions because their stiffness can be precisely tuned by varying the ratio of acrylamide to bis-acrylamide5,6. Compared to other substrates such as collagen-coated glass or commercial hydrogels, PA gels offer independent control over stiffness and biochemical ligand density, enabling systematic dissection of mechanical cues. Although several protocols exist for PA gel fabrication7,8,9, they often lack detailed optimization for specific cell types, particularly for rare primary cells like SLCs.

Here, we present a robust and reproducible protocol for preparing PA hydrogels with defined stiffness (1–100 kPa) tailored for culturing mouse SLCs. The method includes step-by-step instructions for gel casting, swelling equilibration, surface functionalization with Sulfo-SANPAH, and collagen coating to promote cell adhesion. By following this protocol, researchers can generate substrates with tunable stiffness (ranging from 1 to 100 kPa) that mimic the mechanical environment of young (soft) and aged (stiff) testes, enabling quantitative investigation of stiffness-dependent SLC responses. The system is also adaptable to other mechanosensitive cell types and provides a platform for drug screening targeting stiffness-related pathologies.

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Protocol

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All animal procedures were approved by the Institutional Animal Care and Use Committee of Sun Yat‑sen University (Approval No. SYSU-IACUC-2026-B1278) and were performed in accordance with the institutional guidelines.

1. Isolation and culture of primary mouse SLCs

  1. Dissect testes from C57BL/6 mice and carefully remove the tunica albuginea.
  2. Mince the testes into small pieces.
  3. Dissociate interstitial cells from seminiferous tubules by incubating in 1 mg/mL collagenase type IV in DMEM/F12 at 37 ºC for 15 min.
  4. Add DMEM/F12 containing 10% fetal bovine serum to stop collagenase activity.
  5. Centrifuge at 1500 × g for 3 min at room temperature.
  6. Resuspend the pellet in PBS and filter through a 70 µm filter.
  7. Enrich CD51⁺ cells by fluorescence-activated cell sorting (FACS) using an Influx Cell Sorter.
  8. Seed the enriched cells in SLC culture medium composed of DMEM/F12 supplemented with: 1 nM dexamethasone, 1 ng/mL LIF, 5 µg/L insulin‑transferrin‑sodium selenite, 5% chicken embryo extract, 0.1 mM β‑mercaptoethanol, 1% nonessential amino acids, 1% N2, 2% B27, 20 ng/mL basic fibroblast growth factor, epidermal growth factor, platelet‑derived growth factor, and oncostatin M.
  9. Culture the SLCs under standard conditions (37 °C, 5% CO₂) until they reach the desired density for seeding onto hydrogels.

2. Assembling the gel casting glass container

  1. Carefully inspect and clean the specialized glass plates and spacers used for casting polyacrylamide gel electrophoresis (PAGE) gels, ensuring they are free of dust, damage, and residues.
  2. Correctly assemble the glass plates, spacers, and clamps according to the manufacturer's instructions, ensuring the assembly is well-sealed to prevent leakage during gel casting.
  3. Place the assembled glass container securely on a laboratory stand, ready for casting.
    NOTE: The casting setup uses standard Western blot (sodium dodecyl sulfate [SDS]-PAGE) glass plates with fixed spacers of either 1.0 mm thickness, ensuring reproducible gel thickness and a flat surface for cell culture.

3. Preparing PAGE gel mix solution

  1. Precisely measure the following reagents according to the experimental design (see Table 1) into a 15 mL or 50 mL sterile centrifuge tube: 40% Acrylamide stock solution, 2% Bis-acrylamide stock solution, 1M HEPES buffer (pH 8.5), Sterile ddH₂O.
    CAUTION: Acrylamide and bis‑acrylamide are neurotoxins. Always wear gloves and a dust mask when weighing dry powder to avoid skin contact and inhalation of airborne particles. Procedures should be performed within a fume hood.

4. Adding initiator and catalyst, and casting the gel

  1. Add the following to the mixed solution sequentially: 10% Ammonium Persulfate (APS): Acts as the initiator to start the polymerization reaction. N,N,N',N'-Tetramethylethylenediamine (TEMED): Acts as the catalyst to accelerate the polymerization reaction. For a total gel volume of 6 mL, add 60 µL of 10% APS and 6 µL of TEMED (see Table 1 for scaling).
    NOTE: The polymerization reaction begins immediately after adding TEMED; therefore, subsequent steps must be performed swiftly.

5. Pouring the mixed solution

  1. Immediately pipette or pour the mixed solution steadily along one edge of the glass container to avoid creating bubbles.

6. Allowing the gel to polymerize

  1. Let the cast gel container sit undisturbed at room temperature.
    NOTE: Polymerization usually takes 15–30 min at room temperature (20–25 °C).
  2. Proceed to the next step once a clear interface between the unpolymerized gel mixture and the polymerized gel is visible and the gel is completely solid (the gel does not flow when the container is tilted).
  3. Immediately after casting, carefully overlay a thin layer of absolute ethanol (or water-saturated ethanol) on top of the gel mixture to exclude atmospheric oxygen, which inhibits radical polymerization. The ethanol also helps form a flat upper surface.
  4. After polymerization, remove the ethanol before disassembling the plates.

7. Disassembling the container and harvesting the gel

  1. Carefully disassemble the clamps and use a plastic wedge or spatula to gently pry the glass plates apart, allowing the polymerized PAGE gel to remain intact on one plate.
  2. Prepare a culture dish containing an ample amount of sterile PBS.
  3. Carefully peel the gel from the glass plate using a spatula or gloved hand, and let it slide smoothly into the PBS.
  4. Seal the dish containing the gel in PBS and incubate at 4 °C overnight.
    NOTE: This step is crucial. The newly prepared gel is dehydrated and must fully absorb water and swell to its final dimensions in PBS. If this step is skipped and the gel is cut directly, it will continue to expand in subsequent cell culture medium, likely exceeding the area of the culture well and rendering it unusable. The gel thickness after swelling is 1 mm. This is critical because when the gel thickness falls below 100 µm, cells may sense the stiffness of the underlying rigid culture plate, which would interfere with the intended mechanobiological measurements.

8. Cutting and transferring the gel to a culture plate

  1. The next day, retrieve the gel from 4 °C. Using a sterile biopsy punch or blade cutter (with a diameter matching the well size of the culture plate, e.g., 6-well plate), cut the gel under sterile conditions.
  2. Within a biosafety cabinet, use sterile forceps to gently pick up the cut gel disc and place it in the center of an empty, sterile culture well.

9. Initial washing and UV irradiation

  1. Add sufficient sterile PBS to the well containing the gel, ensuring it is completely submerged.
  2. Gently rock the culture plate to wash the gel surface.
  3. Aspirate the PBS using a pipette.
  4. Repeat this washing process once more, for a total of two washes, each lasting 3 min.
  5. After washing, add sufficient sterile PBS to cover the gel again. Place the entire culture plate with the lid slightly ajar under a UV lamp (inside a biosafety cabinet or a dedicated UV crosslinker) and irradiate for 1 h for basic sterilization.

10. Activation of Sulfo-SANPAH crosslinker

  1. Inside the biosafety cabinet, carefully aspirate the PBS from the well.
  2. Before aspirating, gently separate the gel from the well walls and bottom using a pipette tip to avoid damaging the gel due to liquid surface tension.
  3. Transfer the gel to another clean well in the same culture plate using sterile forceps.
    NOTE: When transferring the gel, first adding a small amount of PBS to the clean well can help expel air bubbles trapped between the well bottom and the gel upon placement, and also serves as an additional wash.
  4. Prepare crosslinker working solution: Freshly prepare a 0.2 mg/mL Sulfo-SANPAH working solution by diluting the stock solution (see Table 1) using sterile water or the recommended buffer (e.g., PBS).
    NOTE: Protect the solution from light.
  5. Add sufficient Sulfo‑SANPAH working solution to cover the gel (e.g., 250 µL for a 12‑well plate, 500 µL for a 6‑well plate), ensuring the gel is completely covered.
  6. Place the plate under 365 nm wavelength /120 mJ/cm2 UV light and irradiate for 1 h.
    NOTE: This step activates Sulfo-SANPAH, enabling it to bind to functional groups on the gel surface.

11. Crosslinker activation and final washes

  1. After irradiation, aspirate the Sulfo-SANPAH solution from the well inside the biosafety cabinet.
  2. Add sufficient sterile PBS to the well, gently rock to wash the gel surface, and aspirate the PBS.
  3. Repeat this washing process once more, for a total of two washes, each lasting 3 min, to thoroughly remove any unreacted Sulfo-SANPAH.

12. Preparing rat tail type I collagen working solution

  1. Use a 0.02 M acetic acid solution as a solvent to dilute the rat tail type I collagen stock solution.
  2. Adjust the final working solution concentration to 60–100 µg/mL. For example, if the collagen stock concentration is 4 mg/mL, add 15–25 µL of stock to 985–975 µL of 0.02 M acetic acid to obtain 1 mL of working solution.

13. Collagen coating and incubation

  1. Add the appropriate volume of collagen working solution to each well containing the activated gel according to the plate type: add 2 mL for a 6-well plate, or 1 mL for a 12-well plate.
  2. Gently swirl the culture plate to ensure the collagen solution evenly covers the gel and the well bottom.
  3. Cover the plate and incubate overnight in a 37 °C, 5% CO₂ incubator to allow the collagen to fix onto the gel surface via Sulfo-SANPAH crosslinking.

14. Secondary UV irradiation and fixation

  1. The next day, remove the plate and irradiate again under about 120 mJ/cm2 UV light for 1 h.

15. Remove unbound collagen and seed cells

  1. Inside the biosafety cabinet, carefully aspirate the rat tail type I collagen working solution from the wells.
  2. Add sterile PBS to the wells, gently rock to wash the gel surface, and aspirate the PBS.
  3. Repeat the wash once more, for a total of two washes, each lasting 3 min.
  4. After washing, the gel matrix is ready. Resuspend the prepared stem Leydig cells in the complete SLC culture medium (composition detailed in step 1).
  5. Seed the cell suspension directly onto the gel surface. The recommended seeding density is 2 × 104 cells/cm2 (e.g., approximately 2 × 105 cells per well for a standard 6-well plate).
  6. Incubate the culture plates at 37 °C in a humidified 5% CO₂ incubator.
  7. To maintain optimal cell viability and steroidogenic function, change the culture medium every 48 h.

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Results

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Successful execution of this protocol yields polyacrylamide hydrogels with defined stiffness (ranging from 1 to 100 kPa) that remain firmly attached to the culture plate and support robust SLC adhesion and spreading. Figure 1 provides a schematic overview of the entire workflow, from gel casting to cell seeding, enabling users to visualize the key stages of the protocol.

Mechanical validation of polyacrylamide hydrogels (target stiffness: 1, 5, 15, 30, 50, and 100...

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Discussion

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The mechanical properties of the extracellular matrix play a fundamental role in regulating stem cell behavior, yet the tools to systematically study these effects in reproductive cells remain limited. Our previous work demonstrated that pathological matrix stiffening during aging disrupts stem Leydig cell (SLC) homeostasis through the Piezo1/ROS/Gli1 axis, leading to testosterone decline10. Building on this discovery, we developed this polyacrylamide hydrogel protocol to provide a standardized, r...

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Disclosures

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The authors have nothing to disclose.

Acknowledgements

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The funding for this project was provided by the National Key Research and Development Program of China Stem Cell and Translational Research(2021YFA1100601), National Natural Science Foundation of China (82371608), Guangdong Basic and Applied Basic Research Foundation (2023B1515020016), and Shenzhen Fundamental Research Program (JCYJ20240813150417024, JCYJ20240813150422030).

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Materials

List of materials used in this article
NameCompanyCatalog NumberComments
Acetic acidSigma-AldrichCat#A6283Diluent for rat tail collagen (0.02 M)
Acryiamide   Sangon BiotechCat#A100341-0500Monomer for polyacrylamide gel preparation
Ammonium persulfate (APS) Sangon BiotechCat#A100486-0100Initiator for gel polymerization
B27 supplementInvitrogenCat#A1486701Defined supplement enriched for antioxidants and hormones; supports neuronal and stem cell survival (2% v/v)
Basic fibroblast growth factor (bFGF)InvitrogenCat#13256029Mitogenic growth factor; promotes SLC proliferation and stemness (20 ng/mL)
Bis-acrylamide Shanghai yuanye Bio-TechnologyCat#S14002Crosslinker for polyacrylamide gels
Chicken embryo extractUS BiologicalsCat#C3999Rich source of growth factors and nutrients; supports SLC growth and viability (5% v/v)
Collagen, Type I, from rat tailYEASENCat#40125ES50Coats the Sulfo-SANPAH-activated polyacrylamide hydrogel surface to promote SLC adhesion and culture.
Collagenase Type IVGibcoCat#17104-0191 mg/mL in DMEM/F12 for testicular tissue digestion
CYP11A1 antibodyGeneTexCat#GTX56293For western blotting
DexamethasoneSigma-AldrichCat#D1756Glucocorticoid receptor agonist; supports SLC proliferation and stemness maintenance (1 nM)
DMEM/F12 mediumGibcoCat#11320033Basal medium for digestion, washing, and SLC culture
Epidermal growth factor (EGF)PeproTechCat#AF-100-15Stimulates SLC proliferation and maintains undifferentiated state (20 ng/mL)
Fetal Bovine Serum (FBS)VISTECHCat#SE100-011Used at 10% to stop collagenase activity
FijiN/Ahttps://imagej.net/FijiImage analysis software
GADPH antibodyProteintechCat#60004-1-IgFor western blotting
Gel digestion enzymes Accurate BiotechnologyCat#GXDLFAEnzyme mixture for testicular tissue digestion and SLC isolation
HEPES CytivaCat#SH30237.01Buffer to maintain pH 7.0–7.4
HSD3β antibodySanta CruzCat#sc-515120For western blotting
Influx Cell SorterBDhttps://www.bdbiosciences.com/content/dam/bdb/marketing-documents/BD_Influx_tech_specs.pdf
Insulin-Transferrin-Sodium Selenite (ITS)Sigma-AldrichCat#11074547001Promotes cell survival, glucose uptake, and antioxidant defense (5 μg/L)
KnockOut serum replacement (KSR) GibcoCat#10828-028Serum substitute for SLC culture medium
LIF (Leukemia Inhibitory Factor)MilliporeCat#LIF1010Cytokine that maintains stem cell pluripotency and self-renewal (1 ng/mL)
Mice testiclesThis paperN/AIsolated from C57BL/6 mice
Mouse Testosterone ELISA KitFine BiotechCat#40203ES80For quantification of testosterone in culture supernatants
Mouse: C57BL/6 Shenzhen TopBiotechN/AMouse strain used for testis collection
Mouse: Testicular Stem Leydig Cells (SLCs) This paperN/APrimary cells isolated from mouse testes
N2 supplementInvitrogenCat#17502001Defined serum-free supplement supporting neural and stem cell cultures (1% v/v)
Non-essential amino acidsHyCloneCat#SH30050.03Provides nitrogen sources for protein synthesis and cell metabolism (1% v/v)
Oncostatin M (OSM)PeproTechCat#300-10TCytokine involved in SLC differentiation regulation and Leydig cell maturation (20 ng/mL)
Phosphate-Buffered Saline (PBS)GibcoCat#10010023Washing and resuspension buffer
Platelet-derived growth factor (PDGF)PeproTechCat#100-14BSupports cell proliferation, migration, and survival (20 ng/mL)
Prism 9.0GraphPadhttps://www.graphpad.com/Software for statistical analysis and graphing
StAR antibodyProteintechCat#67130-1-IgFor western blotting
Sulfo-SANPAH MACKLINCat#102568-43-4Heterobifunctional crosslinker for gel surface activation
TEMED PhygeneCat#PH0341Catalyst for polymerization
β-MercaptoethanolInvitrogenCat#21985023Reduces oxidative stress and supports cell growth in culture (0.1 mM)

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Tags

Polyacrylamide HydrogelsMatrix StiffnessStem Leydig CellsExtracellular MatrixHydrogel FabricationCollagen CoatingSubstrate StiffnessCell DifferentiationMechanobiologySteroidogenic Function

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