Journal of Minerals & Materials Characterization & Engineering, Vol. 11, No.4, pp.427-435, 2012
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Spectroscop ic Analysis of Expired and Pure Melmet
R.Kayalvizhia*, M.Sri Vidhya Rubinia, A.Christy Ferdinanda, G.Meenakshib
aDepartment of Physics, St.Joseph’s College of Arts & Science, Cuddalore.
bDepartment of Physics, K.M.C.P.G.S, Pondicherry.
*Corresponding Author: firstname.lastname@example.org
Spectroscopy is a perfect analyzer to find the elements of all matter. The application of
spectroscopy has been used to interpret the effect of antibiotics and other medicines after its life
duration. This has been studied by using the diabetics tablet melmet, expired for an year, to
visualize the changes physically and chemically [1-3]. It has been observed that the occurrence
of changes in color and r eduction of smell and als o the formation of new peaks and shift b y XRD
and UV, FTIR characterization respectively .
Keywords: UV – Ultraviolet–Visible Spectroscopy , FTIR - Fourier Transform Infrared
Spectroscopy, XRD – X-ray diffraction, DSC - Differential Scanning Calorimetry
In this new era medicine plays a vital role to human beings else for all living beings by healing
diseases. In that Melmet (metformin hydrochloride) plays a vital role in treatment of diabetics
and poly cystic ovary diseases. Melmet contain metformin which is used for glucose tolerance
and the chances increase of fertility. It helps to control blood sugar level. PCOD (Polycystic
Ovar y Diseas e) occur due to imbalance or abnormality in the hormones which can be control by
Many people especially who are living in remote areas consuming the medicine even after the
expi r y date due t o t he lack of k no wledge in t he medical fi eld . H en ce, i t i s es sen ti al t o ed ucate th e
428 R.Kayalvizhi , M.S ri Vidhya Rubini Vol.11, No.4
village people about the effect of consuming medicine after the expiry date. It is desired to take
up some medicine after the expiry date to investigate their changes in physical and chemical
properties . One of s uch m edici ne was Melmet , it is used for t he tr eatm ent o f diabet ics. Since,
most of the human beings are suffering by this disease, that Melmet drug can be harmful to
health i n several ways aft er expir y [7, 8]. For this Melmet was made to cross its life duration for
one year. This has been done b y keeping it in an undisturbed p lace at nor mal room tem perature.
After that the pure Melmet and expired Melmet has been analyzed by Spectroscopic technique
such as XRD, UV, FTIR, and thermal analysis DSC.
The X-ray Diffractometer analysis has been carried out for the rapid identification and
quantification of material by using Diffractometer system of XPERT-PRO at 2 theta position of
10.088 to 79.9381 2 with CuKα.
15 20 25 30 35 40
15 20 25 30 35 40 45
Fig.1 (a) and (b) shows the XRD analysis peak for pure
and expired Melmet sample
The optical absorption and transmission spectra have been recorded by using UV-VIS_NIR
spectrometer in the range from 190-370nm as shown in Figure 1(a) and 1(b).
Vol.11, No .4 SPECTROSCOPIC ANALYSIS OF EXPIRED 429
Fig.2 (a) and (b) shows the UV analysis peak for unexpired and expired Melmet sample
A non-destructive technique of FT-IR spectrometer has been made for pure and expired sample
for around 3gm of drug mixed with KBr powder in the range of 4000-400cm-1. The FT-IR
spectrum for absorption and transmission has been shown in Table 1, Figure 2(a), (b) and 3(a),
Table 1. Functional group and IR absorption bands.
Functional group IR absorption bands (cm-1)
Pur e Impure
N-H Asymmetric stretching
C-H Asymmetric stretching
N-H Symmetric stretching
Strongly bonded Hydrogen
vibrations 2691.5 2691.0
C=C Asymmetric ring
stretching 1578.5 1575.0
C-N Asymmetric stretching
C-N Symmetric stretching
N-H in –plane bending
C-H out of plane bending
430 R.Kayalvizhi , M.S ri Vidhya Rubini Vol.11, No.4
Fig 3 (a) & (b) shows the transmittance and absorbance peak for pure sample
Vol.11, No .4 SPECTROSCOPIC ANALYSIS OF EXPIRED 431
Fig 4 (a) & (b) shows the transmittance and absorbance peak for expired sample
432 R.Kayalvizhi , M.S ri Vidhya Rubini Vol.11, No.4
Differential Scanning Calorimetry has been used to measure the amount of h eat energy absorbed
(endothermic) or released (exother mic) by the drug when it is heated or cooled processes.
Fig 5 (a) & (b) DSC endothermic curve for pure and expired sample
Vol.11, No .4 SPECTROSCOPIC ANALYSIS OF EXPIRED 433
Expired drugs can be harmful to health in several ways; they can be unpredictable in
effectiveness, simply ineffective, or even toxic.
According to the pharmaceutical industry, there are certain medications, such as nitroglycerine
(used by heart patients for chest pain), insulin (used by diabetics to control blood sugar), and
liquid medications such as antibiotics that degrade more quickly than other medications. This
means that some of the effectiveness of the medication is lost, if it is used after the expiry date.
In some cases risk with heart disease, diabetes, or serious infection. And while much of the
original potency remains in other medications if used beyond their expiry date, their
effectiveness depends in large part upon how the medication is stored. Factors shorten the
lifespan of drug are moisture, increased temperature, manufacturing impurities, and, for some
drugs, light and so on. Here the expired sample and unexpired sample were characterized by
using XRD and UV to clarify why they are harmful after crossing the expiry date.
The excitation of X-ra y in the life time crossed melmet (Fig 1a & 1b) has been found that in an
expired sample some elements were newly raised. While comparing unexpired sample with
expired drug the 2 theta values were incr eased slightl y and correspondin gly th e d-spacing range
also decr eased in fr action. This is due to the incorporation of some other m aterial in the original
sample. The formation of new 211 planes has been seen in expired drug. The pyramidal plane
113 where dominated 112 pyramidal plane and 003 basal more in expired drug. i.e 112 and 003
planes have been compressed and 110 planes too. The decrease d-spacing values resulting that
the drug molecule getting compress. And so it is not easy to get it diluted soon. Because of this
condition it is contaminate in the kidney and developing a serious risk such as heart disease,
diabetes, or serious infection.
From UV absorption pattern (Fig 2a & 2b) it is found that in an unexpired sample the two
absorption peaks have been seen. First peak is around at 191nm with an absorbance range of
0.166 and the second peak is around 235nm with an absorbance range of 0.133. Whereas in an
expired sample the absorbance range is slightly shifted above to 0.200 and 0.166 absorbance
The complexity of infrared spectra in 1450 to 600 cm-1 (Fig 4 a & 4 b) region makes it difficult to
assign all the absorption bands, and because of the unique patterns found there, it is oft en called
the fingerprint region. Absorption bands in the 4000 to 1450 cm-1 region are usually due to
stretching vibrations of diatomic units, and this is sometimes called the group frequency region.
A symmetric is a fashion at a wave number of 3173.6 cm-1, 3178.0cm-1, 1419.8cm-1, 1418.0cm-1,
in which both bonds lengthen and contract together (in-phase), and the other in an asymmetric
434 R.Kayalvizhi , M.S ri Vidhya Rubini Vol.11, No.4
fashion, in which one bond shortens while the other lengthens. The asymmetric stretch at a wave
number of 3369.7cm-1, 3371.7cm-1, 3295.0 cm-1, 3293.1 cm-1, 1480.9 cm-1, 1482.1 cm-1 is
infrared active because there is a change in the molecular dipole moment during this vibration.
(To be "active" means that absorption of a photon to excite the vibration is allowed by the rules
of quantum mechanics.) .
Bond stretching 2182.2 cm-1 and bond bending 735.0 cm-1, 734.4 cm-1, more complicated
molecules vibrate in rocking and twisting modes, which arise from combinations of bond
bending in adjacent portions of a molecule.
Torsions at 1629.5 cm-1, 1634.3 cm-1 involve changes in dihedral angles. This type of mode is
analogous to twisting the lid off the top of a jar. No bonds are stretched, and no bond angles
change, but the spatial relationship between the atoms attached to each of two adjacent atoms
will ch ange. [ 10] Stretching frequencies are higher than corresponding bending frequencies. (It is
easier to bend a bond than to stretch or compress it.)At a wavenumber of 2691.5 cm-1, 2691.0
cm-1, a strong bond to hydrogen have higher stretching frequencies than those to heavier atoms.
Triple bonds have higher stretching frequencies than corresponding double bonds, which in turn
have higher frequencies than single bonds.
In a rocking, wagging or twisting coordinate the bond lengths within the groups involved do not
change which is at 798.9 cm-1, 798.8 cm-1. The angles do. Rocking is distinguished from
wagging by the fact that the atoms in the group stay in the same plane. 
Fig (5a & 5b) shows that the thermal analysis of pure and expired medicine. Pure melmet has
been started to characterize from 10°C to 500°C for an amount of 5mg in Ramp method. The
endothermic peak has been start at 225.59°C after the Glass Transition and exists its melting
point at 230.20°C. After endothermic peak its starts to dispose in the form of brown colour. The
same endothermic peak has been found in expired melmet but at high heat flow level. Cooling
curve were tried to find its exothermic process but there is no result since it’s not a crystalline
The experimental data indicates that the medicine which crossed its life time develops some new
element which causes the chan ges in its ph ysical and chemical condition. Using Xrd it’s clearly
found that the incorporation of elements in the form of new peak and shift in absorption peak
explains its molecular contraction after expiry. And the small changes in its Stretching condition
using FTIR and the shift in Heat Flow during Endothermic process explain the changes in its
molecular bonding strength.
Vol.11, No .4 SPECTROSCOPIC ANALYSIS OF EXPIRED 435
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