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Recent development on porous calcium phosphate ceramics for biomedical application

Sopyan I

Med J Malaysia, 2008 Jul;63 Suppl A:14-5.
PMID: 19024961

Porous calcium phosphate ceramics have found enormous use in biomedical applications including bone tissue regeneration, cell proliferation, and drug delivery. In bone tissue engineering it has been applied as filling material for bone defects and augmentation, artificial bone graft material, and prosthesis revision surgery. Their high surface area leads to excellent osteoconductivity and resorbability providing fast bone ingrowths. Porous calcium phosphate can be produced by a variety of methods. This paper discusses briefly fundamental aspects of porous calcium phosphate for biomedical applications as well as various techniques used to prepare porous calcium phosphate.
Porous alumina-hydroxyapatite composites through protein foaming-consolidation method

Sopyan I, Fadli A, Mel M

J Mech Behav Biomed Mater, 2012 Apr;8:86-98.
PMID: 22402156 DOI: 10.1016/j.jmbbm.2011.10.012

This report presents physical characterization and cell culture test of porous alumina-hydroxyapatite (HA) composites fabricated through protein foaming-consolidation technique. Alumina and HA powders were mixed with yolk and starch at an adjusted ratio to make slurry. The resulting slip was poured into cylindrical shaped molds and followed by foaming and consolidation via 180 °C drying for 1 h. The obtained green bodies were burned at 600 °C for 1 h, followed by sintering at temperatures of 1200-1550 °C for 2 h. Porous alumina-HA bodies with 26-77 vol.% shrinkage, 46%-52% porosity and 0.1-6.4 MPa compressive strength were obtained. The compressive strength of bodies increased with the increasing sintering temperatures. The addition of commercial HA in the body was found to increase the compressive strength, whereas the case is reverse for sol-gel derived HA. Biocompatibility study of porous alumina-HA was performed in a stirred tank bioreactor using culture of Vero cells. A good compatibility of the cells to the porous microcarriers was observed as the cells attached and grew at the surface of microcarriers at 8-120 cultured hours. The cell growth on porous alumina microcarrier was 0.015 h(-1) and increased to 0.019 h(-1) for 0.3 w/w HA-to-alumina mass ratio and decreased again to 0.017 h(-1) for 1.0 w/w ratio.
Synthesis and characterization of magnesium doped biphasic calcium phosphate

Toibah AR, Sopyan I, Mel M

Med J Malaysia, 2008 Jul;63 Suppl A:83-4.
PMID: 19024995

The incorporation of magnesium ions into the calcium phosphate structure is of great interest for the development of artificial bone implants. This paper investigates the preparation of magnesium-doped biphasic calcium phosphate (Mg-BCP) via sol gel method at various concentrations of added Mg. The effect of calcinations temperature (ranging from 500 degrees C to 900 degrees C) and concentrations of Mg incorporated into BCP has been studied by the aid of XRD, TGA and infrared spectroscopy (IR) in transmittance mode analysis. The study indicated that the powder was pure BCP and Mg-BCP with 100% purity and high crystallinity. The results also indicated that beta-tricalcium phosphate (beta-TCP) phase can be observed when the powder was calcined at 800 degrees C and above.
A novel hydrothermal process to produce hydroxyapatite powders

Sopyan I, Rosli A, Raihana MF

Med J Malaysia, 2008 Jul;63 Suppl A:81-2.
PMID: 19024994

A novel hydrothermal process has been developed various hydroxyapatite(HA) powder. The HA powder was investigated in different calcination temperatures over the range of 200 degrees C-800 degrees C. TG/DTA and XRD analysis revealed that at temperatures of 700-800 degrees C the decomposition processes and phase changes took place. It is due to the appearance of TCP phase substituting the HA phase. FESEM observation showed that the produced hydroxyapatite powder was extraordinarily fine with nanosize primary particles and almost evenly spherical in shaped. Its high purity proved that the powder fulfills medical requirement.
Cell attachment study of chicken fibroblast cell (DF-1) using ceramic microcarrier granule in bioreactors

Mel M, Sopyan I, Nor YA

Med J Malaysia, 2008 Jul;63 Suppl A:18-20.
PMID: 19024963

Tricalcium phosphate ceramic microcarrier has been developed and introduced to a new possibility for the culture of anchorage dependent animal cells of DF1. It was observed that the number of attached cells was increased with shorter time for both spinner vessel and stirred tank (ST) bioreactor. For those bioreactors, the total viable cell number that had been obtained is about 1.2 x 10(5) cell/ml.
Synthesis and characterization of strontium-doped hydroxyapatite powder via sol-gel method

Mardziah CM, Sopyan I, Hamdi M, Ramesh S

Med J Malaysia, 2008 Jul;63 Suppl A:79-80.
PMID: 19024993

Improvement of the mechanical properties of hydroxyapatite (HA) can be achieved by the incorporation of metal. In addition, incorporation of strontium ion into HA crystal structures has been proved effective to enhance biochemical properties of bone implant. In this research, strontium-doped HA powder was developed via a sol-gel method to produce extraordinarily fine strontium-doped HA (Sr-doped HA) powder. XRD measurement had shown that the powder contained hydroxyapatite phase only for all doping concentration except for 2%, showing that Sr atoms have suppressed the appearance of beta-TCP as the secondary phase. Morphological evaluation by FESEM measurement shows that the particles of the Sr-doped HA agglomerates are globular in shape with an average size of 1-2 microm in diameter while the primary particles have a diameter of 30-150 nm in average.
Influence of manganese doping into HA powders on the properties of its dense bodies

Natasha AN, Sopyan I, Mel M, Ramesh S

Med J Malaysia, 2008 Jul;63 Suppl A:85-6.
PMID: 19024996

The effect of Manganese (Mn) addition on the Vickers hardness and relative density of nanocrystalline hydroxyapatite (HA) dense bodies were studied. The starting Mn doped HA powders was synthesized via sol-gel method with Mn concentration varies from 2 mol% up to 15 mol% Mn. The Mn doped HA disc samples were prepared by uniaxial pressing at 200MPa and subsequently sintered at 1300 degrees C. Characterization was carried out where appropriate to determine the phases present, bulk density, Vickers hardness of the various content of Mn doped HA dense bodies. The addition of Mn was observed to influence the color appearance of the powders and dense bodies as well. Higher Mn concentration resulted in dark grey powders. It was also found that the hardness and relative density of the material increased as the Mn content increased and influenced by the crystallinity of the prepared Mn doped HA powders.
Effect of powder calcination on the sintering of hydroxyapatite

Tan CY, Ramesh S, Aw KL, Yeo WH, Hamdi M, Sopyan I

Med J Malaysia, 2008 Jul;63 Suppl A:87-8.
PMID: 19024997

The sintering behaviour of synthesized HA powder that was calcined at various temperatures ranging from 700 degrees C to 1000 degrees C was investigated in terms of phase stability, bulk density, Young's modulus and Vickers hardness. The calcination treatment resulted in higher crystallinity of the starting HA powder. Decomposition of HA phase to form secondary phases was not observed in all the calcined powders. The results also indicated that powder calcination (up to 900 degrees C) prior to sintering has negligible effect on the sinterability of the HA compacts. However, powder calcined at 1000 degrees C was found to be detrimental to the properties of sintered hydroxyapatite bioceramics.
Sintering behaviour of hydroxyapatite bioceramics

Ramesh S, Tan CY, Aw KL, Yeo WH, Hamdi M, Sopyan I, et al.

Med J Malaysia, 2008 Jul;63 Suppl A:89-90.
PMID: 19024998

The sintering behaviour of a commercial HA and synthesized HA was investigated over the temperature range of 700 degrees C to 1400 degrees C in terms of phase stability, bulk density, Young's modulus and Vickers hardness. In the present research, a wet chemical precipitation reaction was successfully employed to synthesize a submicron, highly crystalline, high purity and single phase stoichiometric HA powder that is highly sinteractive particularly at low temperature regimes below 1100 degrees C. It has been revealed that the sinterability of the synthesized HA was significantly greater than that of the commercial HA. The temperature for the onset of sintering and the temperature required to achieve densities above 98% of theoretical value were approximately 150 degrees C lower for the synthesized HA than the equivalent commercial HA. Nevertheless, decomposition of HA phase upon sintering was not observed in the present work for both powders.
Fulltext In situ ophthalmic gel forming systems of poloxamer 407 and hydroxypropyl methyl cellulose mixtures for sustained ocular delivery of chloramphenicole: optimization study by factorial design

Kurniawansyah IS, Rusdiana T, Sopyan I, Ramoko H, Wahab HA, Subarnas A

Heliyon, 2020 Nov;6(11):e05365.
PMID: 33251348 DOI: 10.1016/j.heliyon.2020.e05365

Background: Conventional drug delivery systems have some major drawbacks such as low bioavailability, short residence time and rapid precorneal drainage. An in situ gel drug delivery system provides several benefits, such as prolonged pharmacological duration of action, simpler production techniques, and low cost of manufacturing. This research aims to get the optimum formula of chloramphenicol in situ gel based on the physical evaluation.
Methods: The effects of independent variables (poloxamer 407 and hydroxypropyl methyl cellulose (HPMC) concentration) on various dependent variables (gelling capacity, pH and viscosity) were investigated by using 32 factorial design and organoleptic evaluation was done with descriptive analysis.
Results: The optimized formula of chloramphenicol in situ gel yielded 9 variations of poloxamer 407 and HPMC bases composition in % w/v as follows, F1 (5; 0.45), F2 (7.5; 0.45), F3 (10; 0.45), F4 (5; 0.725), F5 (7.5; 0.725), F6 (10; 0.725), F7 (5; 1), F8 (7.5; 1), F9 (10; 1). The results indicated that the organoleptic, pH, and gelling capacity parameters matched all formulas (F1-F9), however, the viscosity parameter only matched F3, F6, F8, and F9. Based on factorial design, F6 had the best formula with desirability value of 0.54, but the design recommended that formula with the composition bases of poloxamer 407 and HPMC at the ratio of 8.16 % w/v and 0.77 % w/v, respectively, was the optimum formula with a desirability value of 0.69.
Conclusion: All formulas have met the Indonesian pharmacopoeia requirements based on the physical evaluation, especially formula 6 (F6), which was supported by the result of factorial design analysis.
Fulltext Optimization of ultraviolet ozone treatment process for improvement of polycaprolactone (PCL) microcarrier performance

Samsudin N, Hashim YZH, Arifin MA, Mel M, Salleh HM, Sopyan I, et al.

Cytotechnology, 2017 Aug;69(4):601-616.
PMID: 28337561 DOI: 10.1007/s10616-017-0071-x

Growing cells on microcarriers may have overcome the limitation of conventional cell culture system. However, the surface functionality of certain polymeric microcarriers for effective cell attachment and growth remains a challenge. Polycaprolactone (PCL), a biodegradable polymer has received considerable attention due to its good mechanical properties and degradation rate. The drawback is the non-polar hydrocarbon moiety which makes it not readily suitable for cell attachment. This report concerns the modification of PCL microcarrier surface (introduction of functional oxygen groups) using ultraviolet irradiation and ozone (UV/O3) system and investigation of the effects of ozone concentration, the amount of PCL and exposure time; where the optimum conditions were found to be at 60,110.52 ppm, 5.5 g PCL and 60 min, respectively. The optimum concentration of carboxyl group (COOH) absorbed on the surface was 1495.92 nmol/g and the amount of gelatin immobilized was 320 ± 0.9 µg/g on UV/O3 treated microcarriers as compared to the untreated (26.83 ± 3 µg/g) microcarriers. The absorption of functional oxygen groups on the surface and the immobilized gelatin was confirmed with the attenuated total reflectance Fourier transformed infrared spectroscopy (ATR-FTIR) and the enhancement of hydrophilicity of the surface was confirmed using water contact angle measurement which decreased (86.93°-49.34°) after UV/O3 treatment and subsequently after immobilization of gelatin. The attachment and growth kinetics for HaCaT skin keratinocyte cells showed that adhesion occurred much more rapidly for oxidized surfaces and gelatin immobilized surface as compared to untreated PCL.
Fulltext Comparative Study of In Situ Gel Formulation Based on the Physico-Chemical Aspect: Systematic Review

Kurniawansyah IS, Rusdiana T, Sopyan I, Desy Arya IF, Wahab HA, Nurzanah D

Gels, 2023 Aug 10;9(8).
PMID: 37623100 DOI: 10.3390/gels9080645

In recent years, in situ gel delivery systems have received a great deal of attention among pharmacists. The in situ gelation mechanism has several advantages over ointments, the most notable being the ability to provide regular and continuous drug delivery with no impact on visual clarity. Bioavailability, penetration, duration, and maximum medication efficacy are all improved by this mechanism. Our review systematically synthesizes and discusses comparisons between three types of in situ gelling system according to their phase change performance based on the physicochemical aspect from publications indexed in the Pubmed, ResearchGate, Scopus, Elsevier, and Google Scholar databases. An optimal temperature-sensitive in situ gelling solution must have a phase change temperature greater than ambient temperature (25 °C) to be able to be readily delivered to the eye; hence, it was fabricated at 35 °C, which is the precorneal temperature. In a pH-sensitive gelling system, a gel develops immediately when the bio-stimuli come into contact with it. An in situ gelling system with ionic strength-triggered medication can also perhaps be used in optical drug-delivery mechanisms. In studies about the release behavior of drugs from in situ gels, different models have been used such as zero-order kinetics, first-order kinetics, the Higuchi model, and the Korsmeyer-Peppas, Peppas-Sahlin and Weibull models. In conclusion, the optimum triggering approach for forming gels in situ is determined by a certain therapeutic delivery application combined with the physico-chemical qualities sought.