development method for the preparation kolkheti's sphagnum ... · solution under magnetic...

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Development method for the preparation Kolkheti's Sphagnum Peat

Peloids composite nanoparticles

A. Tsertsvadze, A. Bakuridze, A. Bozkurt, L. Ebralidze, I. Seker

Department of pharmaceutical technology, Tbilisi State Medical University, Georgia

Fatih University / BINATAM (Bio-Nano-Technology R&D Center),Turkey, Istanbul

Abstract:Mud has been successfully used for thousands of years in the treatment of rheumatologic,

neurological disorders and various dermatological pathologies. ,,Peloids” is an internationally

recognized name of all kind medical mud. They are natural mixture of inorganic and organic materials

and performs homogenous, finely dispersed mass with definite physical and chemical properties. Peloids

are predominantly rich with humic substances, which are characterized with high biological activity.

Humic acids stimulate enzymatic activity, regenerative processes and have anti-inflammatory activity.

Besides humic acids peloids contain: amino acids, fatty acids, phenolcarboxylic acids, which are formed

due to degradation of organic compounds. Should be mentioned that there is no data in the literature

about using Kolkheti peat peloids in health care.

While nanotechnology is raising the exciting prospect for drug delivery across the impenetrable skin barrier, preparation Kolkheti's Sphagnum Peat Peloids composite nanoparticle for effective transport of

natural materials is very actual. Nanotechnology is an innovation pacemaker in the development of

health care system.

The review recognize that nanometer sized Kolhketi Sphagnum Peatpeloids particles, can be

incorporated into a polymeric host carrier, in order to enhance diffusion rate of a dispersed material.

Finally preparation method of Kolkheti's Sphagnum Peat Peloids composite nanoparticles is developed

and influence of reagent’s concentration and stirring duration is proved by SEM results. The particles

were found to be spherical, with particle size 20-80 nm as observed from SEM.

I. INTRODUCTION

Application of muds for therapeutic purposes is widely known. Mud has been successfully used for thousands of

years in the treatment of rheumatologic, neurological disorders and various dermatological pathologies

/2/.

Medical muds are natural mixture of inorganic and organic materials and performs homogenous, finely

dispersed mass with definite physical and chemical properties /7,8/. Internationally recognized name of

all kind medical mud is ,,peloids".

Based on their physical and chemical properties peloids are classified into four main types:

1. Silt sulphide;

2. Peat;

3. Sapropel;

4. Pseudocolcanic.

The Kolkheti Lowlands constitute a region of global importance for biodiversity conservation,

especially with respect to its mires and relict forests. The Kolkheti Lowlands (Georgia) is the only

warm-temperate region in the world where sphagnum dominated rain-fed peatlands occur. That’s why

they are called sphagnum peat peloids. Different species of sphagnum contain phenolic compounds,

International Journal of Recent Trends in Engineering & Research (IJRTER) Volume 02, Issue 12; December - 2016 [ISSN: 2455-1457]


carbohydrates, amino acids which obtain broad spectrum of biological action. Composition and

properties of peloids strongly depend on peat forming plants /3,5,10/.

There are seven location of peat peloids spread in Kolkheti region: Churia, Anaklia, Peranga, Chirukhi,

Ispani, Nabada, Imnati. Among them Imnati peat peloids occupies the largest area. There is occurred

unique mire type in Kolkheti Lowlands: the percolation bog with special characteristics with respect to

vegetation, micro-relief, hydrology, and peat stratigraphy /4, 10/.

Peloids are predominantly rich with humic acids, which are characterized with high biological activity.

Humic acids stimulate enzymatic activity, regenerative processes and have anti-inflammatory activity

/5, 6/.

Besides humic acids peloids contain: aminoacids, fatty acids, phenolcarboxylic acids, which are formed

due to degradation of organic compounds.

Peat peloids also contain: chloride, sulfate, carbonate anions, potassium, magnesium, calcium, sodium

cations, microelements, antibiotic like-substances, vitamins and etc.

Peat peloid is considered unique complex of raw materials, high sorption properties of peat,

physiological activity and bactericidal properties provide its utilization in health care.

There is no data in the literature about using Kolkheti peat peloids in health care. That’s why study of

Kolkheti peat peloids is actual in order to determine new application approaches in medicine,

cosmetology and balneology due to their rich and complex composition /1/.

While nanotechnology is raising the exciting prospect for drug delivery across the impenetrable skin

barrier, preparation Kolkheti's Sphagnum Peat Peloids composite nanoparticles for effective transport of

natural materials is very actual. Dermatology and cosmetology is particularly more likely to benefit from

the immense promise it holds. Making nanocompositions from Kolkheti sphagnum peat peloids will

increase their effectiveness by enhancing penetration of minarals and biologically active components of

peat peloids through impermeable skin /9/.

1. Experimental

2.1 Materials

The materilas of the research: Kolkheti sphagnum peat

peloids of different ages (Ispani, Anaklia, Chirukhi, Peranga,

Nabada, Imnati, Churia).

1. Ispani

Sample from - 6.0 m

2. Anaklia

Sample from - 5.0 – 5.5 m

3. Peranga

Sample from – 0.5-1.0m

4. Chirukhi

Sample from – 2.0 – 2.5 m

5. Churia

Sample from – 1.5 -1.8m



1.2. Procedure for preparation

Sample Preparation Process

In the literature we hold there is no data available for nanoparticle preparation methods from peloids.

That’s why preparation methods of clay composite nanoparticles was used and modified, based on their

natural origin. Due to the specific physical, chemical and technological properties of paet peloids

different preparation method was tried and finally modified solvent displacement/precipitation method

was choosed /11, 12/.

15.0 g of each Kolkheti shagnum peat peloids (raw material) was dispersed ultrasonically in 10 ml of

deionized water for 30 min to obtain colloidal network. 70.0 mL of 10% PEG 1500 alcoholic solution

(H2O/C2H5OH – 1/1 V/V ) was prepared. The solution was then poured or injected into an aqueous

solution under magnetic stirring for 1,0-2,0 hour. Then 30,0 ml HCL was added drop by drop (2,0 ml in

each 5 minute) until cloudy solution was formed. Then it was homogenized by Ultra-Turrax 20 000 rpm

for 30 or 60 minutes. The obtained was stirred for 2 or 4 days under magnetic stirring. After this period

pH was measured ≈ 2. Finally, the solvent was removed from the suspensions under heating in drying

cabinet at 80-90 °C till gel similar mass was appeared. Composition of the prepared samples are given in the table below (table 1):

Table 1:

Materials Sphagnum peat

peloids (g)

PEG

1500 (g)

Water

(ml)

H2O/alcohol –

1/1 V/V (ml)

0.1 N HCl

(ml)

0.01 N HCl

(ml)

Ispani 15.0 7.0 10 70 30 -

Ispani A 15.0 7.0 10 70 - 30

Anaklia 15.0 7.0 10 70 30 -

Peranga 15.0 7.0 10 70 30 -

Chirukhi 15.0 7.0 10 70 30 -

Chirukhi A 15.0 7.0 10 70 - 30

Churia 15.0 7.0 10 70 30 -

2.3. Instrumentation

Studies were conducted in Istanbul,Fatih University/BINATAM (Bio-Nano-Technology R&D Center).

Samples were analysed using the following modern instrumental methods:

HR-SEM and EDS/Scanning Electron Microscopy and Energy Dispersive Spectrometry; SEM/EDS –

JEOL JSM-7001F FIELD EMISSION - INCA EDS ANALYSIS SYSTEM; Atomic Force Microscope

(AFM) - XE-100E (Park Systems); Surface Profiler - Nano Map 500LS; DC Sputtering with Carbon

(gold) Coater - Quorum Technologies K550X.

II. RESULTS AND DISCUSSION

At the initial stage of research surface morphology of samples was studied. The same amount of each

sample was placed on the cover slip and dried at room temperature. Surface morphology and roughness

was evaluated by Surface Profiler (Nano Map 500 LS).

The obtained results are given on figures:



Figure 1. 3D Roughness Measurement(Ispani) Figure 2. 3D Roughness Measurement (Anaklia)

Figure 3. 3D Roughness Measurement Figure 4. 3D Roughness Measurement Figure 5. 3D Roughness

Measurement (Chirukhi) (Peranga) (Churia)

As a result of roughness study it was obtained that the Chirukhi sample had the lowest roughness. That’s

why in this sample content of the nanoparticles was analyzed by Atomic Force Microscope (AFM). The

obtained results are given bellow:

Figure 5. AFM Image of Chirukhi

The results show that the sample contains nanoparticles, but they form conglomerates. Therefore must

be mentioned, that due to AFM’s sensitivity towards sample’s roughness for better results it was

recommended to use Scanning Electron Microscopy (SEM ).

The particle size and morphology of samples were analyzed using SEM. The SEM imaging results in

both improved spatial resolution and minimized sample charging and damage due to narrower probing

beam. A thick suspension of peloid nanoparticles were spread on a carbon conductive tape attached to

the surface of SEM brass stub. The particles on the stub were coated with gold. The SEM image of peat

peloid nanoparticles is shown in Figure (figure 6,8,10,12,14,16,17). The particles are spherical in shape

and range of particle size was 20-80 nm.

EDS results confirms elemental composition of the nanoparticles (figure 7,9,11,13,15). Omitting these

peaks are shown in the Table 2,3,4,5,6.



Figure 6. SEM Image of Ispani Figure 7. EDS Image of Ispani

Table2. Elemental Composition table from EDS

Element App Intensity Weight% Atomic%

Conc. Corrn.

C K 14,14 0,2392 39,54 48,34

O K 26,36 0,344 51,22 47

Mg K 0,18 0,6405 0,19 0,12

Al K 3,45 0,7535 3,06 1,67

Si K 5,42 0,81 4,48 2,34

Cl K 0,75 0,677 0,74 0,31

K K 0,27 0,8993 0,2 0,07

Ti K 0,16 0,7372 0,14 0,04

Fe K 0,48 0,7468 0,43 0,11

Totals 100

Figure 8. SEM Image of Anaklia Figure 9. EDS Image of Anaklia

Table3. Elemental Composition table from EDS Element App Intensity Weight% Atomic%

Conc. Corrn.

C K 38,64 0,3895 62,02 68,98

O K 14,17 0,2442 36,29 30,3

Al K 0,22 0,7732 0,18 0,09

Si K 0,56 0,8499 0,42 0,2

S K 0,56 0,7625 0,46 0,19

Cl K 0,7 0,693 0,64 0,24

Totals 100



Figure 10. SEM Image of Peranga Figure 11. EDS Image of Peranga


Conc. Corrn.

C K 16,91 0,305 47,41 55,58

O K 17,33 0,3089 48 42,24

Mg K 0,09 0,6407 0,12 0,07

Al K 1,01 0,7529 1,15 0,6

Si K 2,14 0,8263 2,21 1,11

Cl K 0,62 0,6866 0,77 0,31

K K 0,11 0,9019 0,11 0,04

Ti K 0,07 0,7336 0,08 0,02

Fe K 0,13 0,7407 0,15 0,04

Totals 100

Figure 12. SEM Image of Chirukhi Figure 13. EDS Image of Chirukhi


Conc. Corrn.

C K 7,95 0,1965 31,2 40,06

O K 27,4 0,3859 54,72 52,74

Mg K 0,65 0,6308 0,79 0,5

Al K 2,62 0,741 2,72 1,55

Si K 7,64 0,8056 7,31 4,01

Cl K 0,83 0,6702 0,95 0,41

K K 0,16 0,8992 0,14 0,06

Ca K 0,56 0,8655 0,5 0,19

Ti K 0,13 0,742 0,14 0,04

Fe K 1,5 0,754 1,53 0,42

Totals 100



Figure 14. SEM Image of Churia Figure 15. EDS Image of Churia

Table6. Elemental Composition table from EDS

Element App Intensity Weight% Atomic%

Conc. Corrn.

C K 16,13 0,2723 43,87 52,48

O K 21,35 0,3214 49,17 44,16

Na K 0,12 0,6385 0,14 0,09

Mg K 0,11 0,639 0,13 0,08

Al K 1,8 0,7521 1,78 0,95

Si K 3,45 0,8205 3,12 1,59

S K 0,2 0,7397 0,2 0,09

Cl K 0,65 0,6826 0,71 0,29

K K 0,45 0,9014 0,37 0,14

Ca K 0,08 0,8627 0,07 0,03

Ti K 0,09 0,7352 0,1 0,03

Fe K 0,35 0,7437 0,35 0,09

Totals 100

Figure 16. SEM Image of Ispani A Figure 17. SEM Image of Chirukhi A

3.1. Effect of concentration of reagent and time

Various process parameters such as concentration of HCl and stirring time during the reaction for the

formation of peat peloids composite nanoparticles were studied by varying one parameter and keeping

the other parameters constant.



Concentration of HCl was varied 0.01 N, 30 min homogenization by Ultra-Turax and 2 days under

magnetic stirring. The result obtained by SEM is shown in Figure 16-17, where nanoparticle were not

obtained. Peat peloids composite nanoparticles were formed only when concentration of HCl was 0.1 N

and homogenization time was 60 minute and 4 days under magnetic stirring. The result was as shown in

Figure 6-15.

III. CONCLUSIONS

Based on research we can conclude the following:

Based on research preparation method of Kolkheti's Sphagnum Peat Peloids composite nanoparticles is

developed. While preparing process complying technological conditions is essential. Influence of

reagent’s concentration and stirring duration is proved by results. The peat peloids’ samples prepared using solvent displacement method was found to be nanoparticles. These particles were found to be

spherical. The particle size was 20-80 nm as observed from SEM results. There is no data avaliable in

literature about chemical compostion of Kolkheti sphagnum peat peloids. Therefore a broad spectrum of

chemical elements were observed from EDS results.

Their presence is necessary for the maintenance of certain physicochemical processes which are

essential to life.

Thus, it can be an useful material for dermato-cosmetological application. Due to the complex

composition of Kolkheti sphagnum peat peloids making nanocompositions and target delivery will

contibute range of use peloids medical, cosmetological and balneological practice.

Acknowledgements

The authors are thankful to the staff of R&D Center Bio-Nano-Technology of Istanbul, Fatih University/

BINATAM for collaboration and help.

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