Malays. J. Anal. Sci. Volume 30 Number 4 (2026): 1664

 

Research Article

 

In vitro evaluation of the sun protection factor of Archidendron clypearia extract and optimization of an anti-collagenase serum formula using a simplex lattice design

 

Devi Putri Anggraini, Nabila Julidia Deswita Putri, Supomo*, Yullia Sukawaty, and Eka Siswanto Syamsul

 

Sekolah Tinggi Ilmu Kesehatan Samarinda, 75124 Samarinda, East Kalimantan, Indonesia

 

*Corresponding author: fahmipomo@gmail.com

 

Received: 28 August 2025; Revised: 18 June 2026; Accepted: 14 August 2026; Published: 30 August 2026

 

Abstract

Skin aging is associated with reduced elasticity caused by collagen degradation mediated by collagenase enzymes, and this process is accelerated by ultraviolet (UV) exposure. Natural-based serums are increasingly explored as multifunctional cosmetic products because they may provide both photoprotective and anti-aging effects. This study aimed to evaluate the in vitro Sun Protection Factor (SPF) of the ethanol extract and n-hexane, ethyl acetate, and water fractions of Archidendron clypearia leaf and to optimize an anti-collagenase serum formulation using the Simplex Lattice Design (SLD). The effects of xanthan gum and triethanolamine concentrations on viscosity, spreadability, and pH were evaluated. At 400 ppm, the ethyl acetate fraction showed the highest SPF (38.44 ± 0.05; high), followed by the ethanol extract (33.40 ± 2.28; high), water fraction (21.75 ± 0.23; medium), and n-hexane fraction (8.54 ± 0.07; low). The optimized serum contained 1% xanthan gum and 0.5% triethanolamine and produced a desirability value of 1, viscosity of 1816.67 cPs, spreadability of 5.8 cm², and pH of 7.82. The deviation between predicted and experimental values was below 5%. The optimized serum containing 0.025% extract showed collagenase inhibitory activity with an IC₅₀ of 68.06 ppm. These findings indicate that A. clypearia leaf extract has potential as a natural cosmetic active ingredient; however, reference-controlled SPF testing, stability assessment, in vivo validation, and safety evaluation are required before practical use.

 

Keywords: Archidendron clypearia, collagenase, sun protection factor, simplex lattice design, serum

 


References

1.        Sulistiyowati, A., Yushardi, Y. and Sudarti, S. (2022). Variation in sunscreen sun protection factor (SPF) effectiveness against ultraviolet exposure based on Indonesia’s climatic conditions. Journal of Health Sciences, 12(3): 261–269.

2.        Elsi, Y., Satriadi, T. and Istikowati, T.W. (2020). Ethnobotany of medicinal plants used by the Dayak Meratus indigenous community in Ulang Village, South Hulu Sungai, Kalimantan. Journal of Sylva Science, 03(1): 193–201.

3.        Partomihardjo, T., Hermawan, E. and Pradana, E.W. (2020). Peat Swamp Forest Plants of Merang Kepayang. ZSL Indonesia.

4.        Noviantina, E., Linda, R. and Wardoyo, E.R.P. (2018). Ethnobotanical study of natural cosmetic plants of the Dayak Kanayatn community in Sebatih Village. Protobiont, 7(1): 61–68.

5.        Yuniarsih, N., Indriyati, A. and Munjiani, A. (2021). Review: Herbal face masks in Indonesia. Jurnal Buana Farma, 1(1): 17–21.

6.        Pratiwi, M.W., Wijaya, T.H., Sumayyah, S. and Kurniawan, D.W. (2023). Narrative review: Herbal nanospray as anti-aging. Majalah Farmasetika, 8(3): 267.

7.        Rafique, M. and Hussain Shah, S.N. (2019). Anti-ageing potential of a cream (W/O emulsion) containing grape seed extract: formulation and in vivo evaluation. Journal of Clinical & Experimental Dermatology Research, 10(4): 1–9.

8.        Zofia, N.Ł., Martyna, Z.D., Aleksandra, Z. and Tomasz, B. (2020). Comparison of the antiaging and protective properties of Apiaceae plants. Oxidative Medicine and Cellular Longevity, 2020: 1–16.

9.        Zorina, A., Zorin, V., Kudlay, D. and Kopnin, P. (2022). Molecular mechanisms of dermal extracellular matrix homeostasis alterations induced by ultraviolet radiation and aging. International Journal of Molecular Sciences, 23(12): 1–16.

10.     Carrillo-Norte, J.A. et al. (2024). Anti-aging effects of low-molecular-weight collagen peptide supplementation. Cosmetics, 11(4): 137.

11.     Marbun, F.K., Tarigan, S.B. and Sudarti, S. (2023). Analysis of benefits and impacts of UV radiation on human health. Jurnal Penelitian Inovatif, 3(3): 605–612.

12.     Adzhani, A., Darusman, F. and Aryani, R. (2022). Study on ultraviolet radiation effects on skin. In Bandung Conference Series: Pharmacy, pp. 106–112.

13.     Ayuchecaria, N., Nugroho, W. and Aryzki, S. (2022). SPF determination and physicochemical characterization of Dayak Nanoherbal powder. Journal of Pharmaceutical Care Science, 3(1): 140–146.

14.     Anggreini, D., Saputri, M. and Sari, N. (2024). Understanding SPF value in cosmetics. Jurnal Pengabdian Masyarakat Tjut Nyak Dhien, 3(1): 33–38.

15.     He, H. H., Li, A., Li, S., Tang, J., Li, L., and Xiong, L. (2021). Natural components in sunscreens. Biomedicine & Pharmacotherapy, 134: 111161.

16.     Ji, W., Li, Z., Gu, L., Zou, X., Wu, J., Zhang, S., & Deng, H. (2022). Composition of Archidendron clypearia across harvest periods. SSRN Electronic Journal, 418: 6533.

17.     Ji, W. (2023). Identification of antibacterial and antidiabetic compounds of Archidendron clypearia. Molecules, 28(3): 1–18.

18.     Risman, M. (2022). In vitro and in vivo sunscreen activity of A. clypearia ethyl acetate fraction. Jurnal Penelitian Farmasi Indonesia, 11(1): 32–38.

19.     Hidayah, R. and Nurrosyidah, H.L. (2023). Formulation and stability of grape seed oil serum. Journal of Islamic Pharmacy, 8(1): 34–38.

20.     Sawiji, R.T. et al. (2024). Effect of gelling agent variation on retinoic acid serum. Acta Holistica Pharmaceutica, 6(1): 1–10.

21.     Aprilia, C., Faisal, M. and Prasetya, F. (2022). Formulation and optimization of xanthan gum serum. In Mulawarman Pharmaceuticals Conferences, pp. 30–34.

22.     Suleman, A.W., Wahyuningsih, S., and Puspitasari, Y. (2023). Formulation of antioxidant serum from Syzygium polyanthum extract. Pharmamedica Journal, 8(2): 235–243.

23.     Tsabitah, A. F., Zulkarnain, A. K., Wahyuningsih, M. S. H., and Nugrahaningsih, D. A. A. (2020). Optimization of carbomer, propylene glycol, and TEA in gel formulation. Majalah Farmaseutik, 16(2): 111–118.

24.     Febriani, Y., Lubis, S. H., and Annisa, F. (2022). Formulation of antioxidant serum from red betel leaf extract. Journal of Pharmaceutical Science, 5(1): 120–127.

25.     Purwanto, A., Amrina, F. and Riauwati, R. (2024). Optimization of Euphorbia hirta cream using SLD. Jurnal Insan Farmasi Indonesia, 7(2): 53–65.

26.     Ekawati, A.R., Supriningrum, R. and Handayani, F. (2023). Characterization of ethanol extract of Tabernaemontana macrocarpa leaf. Journal of Pharmaceutical Sciences and Clinical Pharmacy, 20(1): 43–52.

27.     Qomaliyah, E.N., Indriani, N., Rohma, A. and Islamiyati, R. (2023). Phytochemical screening, total flavonoid content, and antioxidant activity of Kalanchoe pinnata leaf. Current Biochemistry, 10(1): 1–10.

28.     Nasution, A.W., Nasution, H.M., Lubis, M.S. and Rahayu, Y.P. (2023). Antibacterial activity of Etlingera elatior leaf fractions against Staphylococcus aureus and Escherichia coli. Journal of Pharmaceutical Science, 6(4): 1488–1497.

29.     Lestari, P., Yusuf, F., Fahdi, F., Tinggi, S. and Kesehatan, I. (2024). Phytochemical screening of Picria fel-terrae leaf using graded maceration. BEST Journal, 7(1): 2249–2255.

30.     Kusumo, D.W., Susanti, Ningrum, E.K. and Makayasa, C.H.A. (2022). Phytochemical screening of secondary metabolites in Carica papaya flower ethanol extract. Journal of Current Pharmaceutical Science, 5(2): 2598–2095.

31.     Aini, S.H., Sabrina, N., Soleha, R. and Lestari, S.M. (2025). Determination of SPF and total phenolic content of Pometia pinnata leaf extracts. Journal of Jamu Indonesia, 10(2): 55–61.

32.     Arifin, B., Nasution, R., Savila, S., Ramadani, R., Helwati, H., Marianne, M., ... and Saidi, N. (2020). Sunscreen activities of Artocarpus heterophyllus bark in lotion formula. Open Access Macedonian Journal of Medical Sciences, 8(A): 461–467.

33.     Rowe, R.C., Sheskey, P.J. and Quinn, M.E. (2009). Handbook of Pharmaceutical Excipients. 6th ed. Pharmaceutical Press, American Pharmacists Association.

34.     Iskandar, B., Putri, R., Wei, C. P., and Renovita, F. (2021). Formulation and antibacterial evaluation of anti-acne serum containing Ocimum africanum leaf extract. Jurnal Buana Farma, 1(4): 14–20.

35.     Yuliani, F., Alfiah, F.B. and Handayani, K.R. (2024). Formulation and physical evaluation of Zingiber cassumunar rhizome emulgel. FARMASAINKES Journal, 4(1): 106–115.

36.     Fitria, N. and Ratu, A.P. (2022). Characteristics and stability of Muntingia calabura fruit extract serum. Pharmamedica Journal, 7(1): 17–27.

37.     Hikmah, F.N., Malahayati, S. and Nugraha, D.F. (2023). Formulation and evaluation of jasmine flower serum gel. Journal of Pharmaceutical Care Science, 3(2): 93–108.

38.     Safaruddin et al. (2024). Formulation and stability study of banana peel extract serum. Inhealth Indonesian Health Journal, 3(2): 172–182.

39.     Setiawan, P.A., Rahmawanty, D. and Sari, D.I. (2023). Formulation of cassava leaf extract serum. Jurnal Pharmascience, 10(2): 394–404.

40.     Fauzah, Noval and Rohama. (2024). Formulation of pumpkin extract serum using xanthan gum. Jurnal Surya Medika, 10(1): 277–287.

41.     Murdiana, H.E., Rahmavika, T. and Rawar, E.A. (2023). Antioxidant serum from lime essential oil using vitamin E. Pharmamedica Journal, 8(2): 209–219.

42.     Fikry, E. et al. (2023). Dermato-cosmeceutical properties of Pseudobombax ellipticum. Saudi Pharmaceutical Journal, 31(10): 1778.

43.     Ananta, M.N.F. et al. (2024). Phytochemical screening of Trigona sp. propolis extracts. Sasambo Journal of Pharmacy, 5(1): 38–45.

44.     Li, D. et al. (2024). Genotype characterization of Archidendron clypearia using microsatellite markers. Forests, 15(7): 1168.

45.     Riasari, H. et al. (2019). Extraction methods and antioxidant activity of Archidendron bubalinum seeds. Pharmacognosy Journal, 11(6): 1278–1284.

46.     Riasari, H., Wibowo, D.P. and Fauzi, N.I. (2022). Hypoglycemic potential of A. bubalinum leaf extract. International Journal of Applied Pharmaceutics, 14(5): 50–55.

47.     Amin, A. and Park, S. (2025). Chemotaxonomy as an efficient tool for medicinal plant identification. Plants, 14(14): 2234.

48.     Nigel, E.E.A. et al. (2023). SPF of Malaysian fruit and vegetable extracts. Malaysian Journal of Chemistry, 25(2): 87–97.

49.     Wardatun, S., Mahyuni, S. and Setiawan, P. (2025). Sunscreen activity of papaya leaf extract fractions. Indonesian Journal of Pharmacy, 5(2): 422–431.

50.     Triyasmono, L. et al. (2025). UV–Vis and chemometric SPF prediction of Acacia leaf extracts. Tropical Journal of Natural Product Research, 9(8): 3854–3859.

51.     Torres-Contreras, A. M. et al. (2022). Plant secondary metabolites against skin photodamage: Mexican plants, a potential source of UV-radiation protectant molecules. Plants, 11(2), 220.

52.     Khaira, Z., Monica, E. and Yoedistira, C.D. (2022). Formulation and physical quality of melinjo seed microemulsion serum. Sainsbertek Journal, 3(1): 299–309.

53.     Ristianti, V., Monica, E. and Aziz, N. (2023). Formulation of an anti-acne serum with citrus essential oil. Sainsbertek Journal, 4(1): 58–65.

54.     Aprilianti, N., Hajrah, H. and Sastyarina, Y. (2020). Optimization of PVA as a gel base. In Mulawarman Pharmaceuticals Conferences, pp. 17–21.

55.     Aisyah, M.N., Purnomo, Y. and Widyaningrum, I. (2022). Role of xanthan gum on physicochemical properties of oleanolic acid gel. Journal of Complementary Medicine Biology, 9(2): 1–5.

56.     Widyartha, G.N.A.Z. et al. (2020). Simplex lattice design for wound dressing gel. Acta Holistica Pharmaceutica, 2(2): 28–36.

57.     Handayani, R., Qamariah, N. and Maretania, J. (2023). Serum formulation from Dioscorea bulbifera tubers. Jurnal Farmasetis, 12(2): 227–236.

58.     Ratnasari, N., Puspariki, J. and Farhan. (2023). Physical stability of cucumber extract serum. Journal of Holistic Health Science, 7(1): 9–16.

59.     Agustiani, F.R.T., Sjahid, L.R. and Nursal, F.K. (2022). Literature review: role of polymers as gelling agents. Majalah Farmasetika, 7(4): 270–287.

60.     Nugrahaeni, F., Srifiana, Y. and Rokhman, A.N. (2021). Effect of xanthan gum concentration on secang hair dye gel. Indonesian Natural Research Pharmacy Journal, 6(2): 29–42.

61.     Lukić, M., Pantelić, I. and Savić, S.D. (2021). Optimal pH for skin and topical formulations. Cosmetics, 8(3): 69.

62.     Widyaningrum, N. et al. (2025). Optimization and antioxidant activity of clay masks. Pharmaceutical Sciences and Research, 12(1): 33–40.

63.     Pratiwi, P.D. and Arnas, D.L. (2024). Simplex lattice optimization of emulsifier in orange peel oil cream. Journal of Clinical Pharmacy and Natural Products, 4(2): 85–93.

64.     Dewi, I.K. et al. (2021). Optimization of ethyl acetate fraction gel from corn cobs. Jurnal Jamu Kusuma, 1(2): 57–66.

65.     Bolton, S. and Bon, C. (2003). Pharmaceutical Statistics: Practical and Clinical Applications. 4th edition. CRC Press.

66.     Wiyono, A.E. et al. (2023). Optimization of CMC-Na and glycerin in tobacco hand sanitizer gel. International Journal of Food, Agriculture and Natural Resources, 4(1): 10–17.

67.     Tanur, E. et al. (2020). FRAP and collagenase inhibition of pineapple core extract. American Scientific Research Journal for Engineering, Technology, and Sciences, 70(1): 99–105.

68.     Aji, A.P., Nurulita, N.A. and Diniatik. (2021). Antiaging activity of purified Azolla microphylla leaf serum. In Prosiding SainTeKes, pp. 159–168.

69.     Piyasena, K.G.N.P.P. et al. (2024). Elastase, collagenase, and tyrosinase inhibition in tea cultivars. Discovery Chemistry, 1: 36.