My P.hD. Days: Supratim

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My P.hD.

Days
Supratim
CeBER SEMINAR 2018/03/05 2

Jadavpur University
Founded in 1955, Jadavpur University is a public research institution situated in the urban area of Kolkata –
formerly Calcutta – in West Bengal.

Its roots date back to 1906 when the National Council of Education was formed in the wake of the local Swadeshi
Movement, a popular uprising against Britain’s plans to partition the land. Today, the university is proud to stand as
a symbol of this movement.

Made up of 36 departments, with 21 interdisciplinary schools and 40 centres of study, it serves roughly 10,000
students. It offers 39 undergraduate programmes, 57 postgraduate, and courses for masters in philosophy, PhDs and
diplomas.

In recognition of its commitment to research and education in the fields of engineering and technology, Jadavpur
University was among 127 institutions to be given financial support by the World Bank through its Technical
Education Quality Improvement Programme.

It was also the first university in India to be accredited by the Nippon Foundation, a Japanese grant-giving
organisation, in recognition of the research undertaken across its social sciences and humanities departments.

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Instrumental facilities at the Department of Metallurgical and Material
Engineering

 Atomic Absortion Spectrophotometer With Graphite Furnace.


 High-Resolution Transmission Electron Microscope.
 Field Emission Scanning Electron Microscope.
 Scanning Electron Microscope with EDS.
 Fourier-transform Infrared Spectrophotometer.
 X-ray Diffractometer Fitted with SAXS.

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Research Areas

Biohydrometallurgical
Extraction of Metals

Synthesis and
characterization of Biological synthesis
silica based drug of metal
delivery system nanoparticles

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Recovery of Metal Values from
Chromite Overburden using
Biohydrometallurgical Treatments
Research Problem
 In spite of it’s complex mineralogy Sukinda chromite overburden finds importance due to it’s nickel
and other metal content.
 The ever-increasing demand of nickel which is imported in India, sets the backdrop of the present
study.
 Along with nickel, bioleaching of another strategic metal cobalt, which is also imported to meet the
domestic demand, will be conducted.

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Aim of the work
•To investigate the leaching efficiency of heterotrophic fungi in recovery of metal values from
Chromite Overburden of Sukinda mines, Orissa.
•To investigate the rate of recovery of metal using one step, two step and culture filtrate
bioleaching.
•To optimize process parameter for better leaching.
•To determine the kinetics of nickel and cobalt recovery using organic acid and fungal culture
filtrate leaching.

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Source and Description of the Ore

The map has been reconstructed using a software (AUTOCAD ver.6) based on a published
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article Banerjee P.K., 1972. Geology and geochemistry of the Sukinda ultramafic field,
Cuttack District, Orissa. Memoirs of the geological survey of India. 103, pp. 1-8.
Overburden of Sukinda chromite mines in Orissa, India is generated in huge amounts
along with the production of chromite ore.
The chromite overburden samples were collected from the major mining site of Kaliapani
open cast mines of Orissa Mining Corporation at Sukinda Valley, Orissa.
 The ore is spread over a stretch of 7 km length from Kansa in the east to Muruabil in the
west.
The ore is highly weathered and is rich in oxides of iron containing minor amounts of
nickel and cobalt.
The nickel is reported to be entrapped in the goethite (FeOOH) matrix and cobalt occurs
primarily in manganese mineral phases.
The chromite overburden contains 0.4% to 1,2% nickel and 0.02% to 0.05% cobalt.
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Methods
Chromite Overburden Production of Fungal Culture
Filtrate Sucrose Medium

Pretreated @ 600° C

Fungal Culture Filtrate Fungal Leaching with


Leaching by One Step, Two Varying Sucrose
Step and Culture Filtrate Concentration (1, 5.5, 10%)
Process @ 2, 5, 8% Pulp
Density

CeBER SEMINAR Study of Fungal Leaching Kinetics Using all Optimized 2018/03/05 12

Parameters
Culture Media
Medium Type Media Constituent Concentration in gm/L

Sucrose 100/55/10

MgSO4 7H2O 0.5


Sucrose Medium
Initial pH-6.8 KH2PO4 1

NH4NO3 3

Yeast Extract 1

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Recovery of Ni and Co using (A) one step bioleaching; (B) two step bioleaching and (C) culture
filtrate bioleaching.
Metal recovery values for the three different bioleaching processes at
three different pulp densities
One Step Bioleaching Two Step Bioleaching Culture Filtrate Bioleaching
Element % Pulp Density % Pulp Density % Pulp Density
Days 2 5 8 2 5 8 2 5 8
7 7.15±0.98 6.52±1.1 2.85±0.87 12.8±1.2 9.36±1.2 4.15±1.3 20.18±2.5 12.69±1.5 7.83±0.97

Nickel 14 16.87±1.47 10.39±2.1 4.54±0.98 31.6±2.3 17.54±2.4 9.35±1.5 53.3±2.1 23.9±2.5 16.45±1.26

21 29.16±2.1 17.41±2.3 9.47±1.4 39.54±2.1 25.49±2.3 11.56±1.8 70.49±2.5 39.95±2.7 20.39±2.4

7 10.71±1.5 5.65±0.98 2.3±0.98 13.05±1.2 10.12±1.2 6.13±1.3 31.3±2.5 18.24±1.5 8.69±1.2

Cobalt 14 24.1±2.3 9.42±1.5 4.45±0.97 27.54±1.4 14.23±1.5 9.45±1.5 40.26±2.1 22.8±1.6 15.73±1.9

21 35.49±2.4 12.41±2.4 6.54±1.1 46.21±2.8 19.34±2.1 12.65±1.8 66.93±2.5 28.74±2.1 19.81±2.2

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Comparison Between Culture Medium
Medium Type Days pH Dry Weight of Fungal Concentration of
Biomass Oxalic Acid in g/L

7 1.7 2.083 3.78


10% Sucrose
14 1.5 3.789 7.54
Medium
21 1.3 4.98 13.54
7 1.8 2.045 1.57
5.5 % Sucrose
14 1.6 3.501 3.47
Medium
21 1.4 3.757 8.67
7 4.5 0.415 0.687
1% Sucrose
14 4.4 1.515 2.87
Medium
21 4.4 1.715 3.05
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Experimental matrix and responses (% metal recovery) for BBD

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ANOVA results of the quadratic model for the recovery of Ni and Co

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The isothermal models tested in this study are presented in
Equations (1)–(12)

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Kinetic Study of Nickel Dissolution

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Kinetic Study of Cobalt Dissolution

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Arrhenius Plot for Nickel

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Arrhenius Plot for Cobalt

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Conclusion
 Culture filtrate bioleaching stood out to be the most effective approach in leaching out both nickel
and cobalt.
 Aspergillus niger strain (NCIM 548) was found to be the most efficient organism for the purpose.
 Dissolution of nickel and cobalt using fungal metabolic acids (oxalic, citric, gluconic) reveals oxalic
acid to be the best among the three.
 Nickel dissolution is diffusion controlled (Ginstling Brounsthein equation) where the process is
regulated by the penetration of organic acid through the porous layers of the iron matrix which
increases with pretreatment.
 Dissolution of cobalt followed mixed model kinetics; first- partly “Shrinking Core model” (spherical
equation) where the ore particle shrinks layer by layer with leaching of the metal in lixiviant solution
upto 1h; it is then followed diffusion controlled kinetics (Ginstling Brounsthein equation) for the rest
of the time period.
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Synthesis and characterization of
silica gel as sustained drug delivery
system

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 Action of pharmaceutical agents is limited by various factors, including their degradation, their
interaction with other cells, and their incapacity to penetrate tissues as a result of their
chemical nature.
 For these reasons, new formulations ( drug + carrier) are being studied to achieve a greater
pharmacological response.
 These systems provide an avenue for controlled drug delivery and proper biodistribution over
a time span.

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 Controlled release systems are designed to deliver
controlled amounts of therapeutic agents to specific target
sites over extended duration of time .

 Controlled release systems aim to improve the effectiveness of drug


therapy. These systems modify several parameters of the drug: the
release profile and capacity to cross biological carriers (depending on
the size of the particle), biodistribution, clearance, and stability
(metabolism), among others.

 Controlled release offers numerous advantages over conventional


dosage forms. This approach increases therapeutic activity and
decreases side effects, thus reducing the number of drug dosages
required during treatment.

 Controlled release methods offer an appropriate tool for site-specific and


time-controlled
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drug delivery. 2018/03/05 27
AIM OF THE WORK

Extraction of medicinal herbal components thereby entrapment of the same in the silica

gel matrix at room temperature and study the mechanism of release estimated under

the influence of different buffer followed by determination of antimicrobial efficacy.

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Advantages of Why
sustained Silica gel?
delivery system

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Preparation of silica gel

TEOS(5ml) +EtOH (5ml) EtOH (5ml) +dH2O(5ml)


taken in a beaker taken in a beaker

Stirred with a magnetic Mixture Stirred with a


stirrer until the solution Added to the TEOS Magnetic stirrer for 30
mixes homogeneously. mixture slowly. min.
Completion of
Kept it 7 -10days
Mixing, sol is packed
For drying.
With a porous cover

highly porous silica Dry, nano porous


gel silica gel obtained.

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Three Herbs are taken.

1. Andrographis paniculata (Kalmegh)

2.Terminalia chebula (Haritoki)

3. Ocimum sanctum (Tulsi)

All three herbs are subjected to extraction by using


chloroform, methanol, distilled water (non-polar to polar
solvent) in soxhlet apparatus.

Extracts are mixed during gel formation.

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Soxhlet extraction apparatus

Condenser

Extraction chamber

Round bottom flask

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Terminalia chebula

Andrographis paniculata

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Ocimum santum

The herbal component is released in biphasic order.

The mechanism of release predominantly follows diffusion and relaxation, Super case-II
transport for first order and zero order equation respectively, diffusion and erosion of the
matrix for Higuchi’s model.

Elution of the extracts from the silica matrix was studied for all the three formulations,
release concentration of extract above the minimum inhibitory concentration (MIC).
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Why
Andrographolide?

Active pharmaceutical ingredient of Andrographis paniculata is andrographolide.

The active or central ingredient in the which causes the direct effect on the disease
diagnosis, prevention, treatment or cure.

Easily obtained in the purest form.

Andrographolide is a diterpene lactone, colourless, crystalline, and bitter in taste and it is


known for anti-parasitic, anti-bacterial, anti-retroviral, anti-diabetic, pro-apoptotic etc.
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Optimization of process parameter

Volume of ethanol Volume of water Temperature of


(mL) (mL) drying C

2 4 35

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Particle size distribution of porous silica

The particles sizes are in a broad range from 1.1 to


2.3 μm for porous silica.
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BET analysis
Sample Surface area Pore Average
name m2/g volume Pore
cm3/g Diameter
(nm)
Silica 900 0.92 2.556

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TEM image of the matrix
Release percentage of Andrographolide in SBF (7.4)

The first release was also greater


than MIC values. A biphasic release
pattern was obtained in which a
sharp release was found in first 4 hs
and subsequent steady and
sustained release obtained in rest
time line.

The release was observed 44.83% in the experimental


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time period.
S1 – 2 mg/kg,
S2 – 8 mg/kg,
S3 – 16 mg/kg

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Different Organ Tissues S1 S2 S3
KIDNEY
Glomerulitis - 2+ 4+
Necrosis of glomerular cell - 2+ 3+
Necrosis of bowman’s capsule - 2+ 4+
Degeneration of convoluted tubules - 2+ 4+

Necrosis of tubular cells - 2+ 4+


Hyperaemia of vessels 2+ 3+ 4+
Black particles 2+ 3+ 4+
LIVER
Degenerative changes - 2+ 4+
Apoptosis - - -
Necrosis - - -
Intercellular space enlargement 1+ 2+ 4+
Black particles 2+ 3+ 4+
SPLEEN
Red pulp changes 1+ 3+ 4+
White pulp changes 1+ 3+ 4+
Black particles 2+ 3+ 4+
LUNG
Alveolar exudate 1+ 2+ 4+
Interalveolar space exudate 1+ 2+ 4+
Hyperaemia of blood vessels 1+ 2+ 4+
Black particles 2+ 3+ 4+
HEART
Degenerative changes - 1+ 1+
Necrotic changes - - -
Hyperaemia of blood vessels - 2+ 3+
Black particles 2+ 3+ 4+
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Mucosal inflammation - 1+ 2+
Ulceration - - -
Black particles 2+ 3+ 4+
Conclusions

 The method for sustained drug release of andrographolide from silica gel matrix which
was prepared using optimized parameters based on BBD design coupled with RSM
methodology.
 The quantitative effect of these factors at different levels on the responses was
predicted by using polynomial equations and high linearity was observed between
predicted and actual values of response variables.
 The S1 silica dose proves to be the most efficient and biocompatible among the three
(S1, S2, S3) which does not show any sign of toxicity or degeneration for an extended
period, while some moderate and prominent changes were found associated with S2

and S3 SEMINAR doses respectively.


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