Analytical Chemistry Letters

ISSN: 2229-7928 (Print) 2230-7532 (Online) Journal homepage: http://www.tandfonline.com/loi/tacl20

Estimation of Anti Diabetic Teneligliptin in

Bulk and Formulation by Densitometric and
Spectrophotometric Method

Sohan S. Chitlange, Diptee G. Rawat & Sejal P. Gandhi

To cite this article: Sohan S. Chitlange, Diptee G. Rawat & Sejal P. Gandhi (2017) Estimation
of Anti Diabetic Teneligliptin in Bulk and Formulation by Densitometric and Spectrophotometric
Method, Analytical Chemistry Letters, 7:4, 556-566, DOI: 10.1080/22297928.2017.1364664

To link to this article: http://dx.doi.org/10.1080/22297928.2017.1364664

Published online: 30 Oct 2017.

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 TACL 7 (4) 2017 pp 556 - 566 556
ISSN Print: 2229-7928
ISSN Online: 2230-7532

Estimation of Anti Diabetic Teneligliptin in Bulk and Formulation

by Densitometric and Spectrophotometric Method

Sohan S. Chitlange*, Diptee G. Rawat and Sejal P. Gandhi

Dr. D.Y. Patil Institute of Pharmaceutical Sciences and Research,
Pimpri, Pune- 411018 (Maharashtra), India
Received 06 June 2016; accepted in revised form 16 April 2017
Downloaded by [University of New England] at 20:54 08 November 2017

Abstract: A simple, accurate, precise and economical HPTLC and UV method has been developed and
validated for the estimation of teneligliptin hydrobromide hydrate (THH) in bulk and tablet dosage form. The
chromatographic method employed pre-coated silica gel 60F254 plates using toluene: methanol: triethylamine
(8:2:0.2 v/v/v) as mobile phase. The plates were developed to a distance of 8.0 cm at ambient temperature.
Experimental conditions such as band size, chamber saturation time, migration of solvent front, slit width, etc
were critically studied and the optimum conditions were selected. A TLC scanner set at 254 nm was used for
direct evaluation of the chromatograms in reflectance/absorbance mode. The system was found to give good
result for Teneligliptin at Rf 0.51. The calibration plot was found linear between concentration range 0.5-3 μg/
band and r2 = 0.9993. Method was validated according to the ICH guidelines. In stability testing, teneligliptin
was found susceptible to alkali hydrolysis and oxidatative degradation. Because the method could effectively
separate the drug from its degradation products, it can be used as a stability indicating method. A UV
spectrophotometric method was also developed using methanol as solvent at λ max 247 nm. Beer’s law was
obeyed in the concentration range of 5-50 μg/ml and r2 = 0.9997. The proposed method was validated according
to the ICH guidelines. Therefore, both the methods and stress degradation study can be used for routine
quality control analysis of Teneligliptin in bulk and pharmaceutical formulation.

Key words: Teneligliptin hydrobromide, HPTLC, spectroscopic method, validation, forced

degradation

Introduction cal regulation of glucose homeostasis. GLP-1 and

Teneligliptin hydrobromide hydrate i.e. {(2S,4S)-
4-[4-(3-Methyl-1-phenyl-1H-pyrazol-5-yl)
piperazin-1-yl] pyrrolidin-2-yl} (1,3-thiazolidin-3-
yl) methanone hemipentahydrobromide hydrate,
is a potent, reversible and selective inhibitor of
the enzyme DPP-4 (Dipeptidyl peptidase 4, EC
3.4.14.5) which is involved in the inactivation of
the incretin hormones (glucagon-like peptide-1
(GLP-1) and glucose-dependent insulinotropic
polypeptide (GIP) 1,2. These incretin hormones are
rapidly degraded by the enzyme DPP-4. Both
incretin hormones are involved in the physiologi-
GIP are secreted by the intestine at a low basal
level throughout the day and concentrations are
increased in response to a meal. GLP-1 and GIP
increase insulin biosynthesis and secretion from
pancreatic beta cells in the presence of normal
and elevated blood glucose levels. Furthermore
GLP-1 also reduces glucagon secretion from pan-
creatic alpha cells, resulting in a reduction in he-
patic glucose production. Teneligliptin binds to
DPP-4 in a reversible manner and thus leads to
an increase and a prolongation of active incretin
levels. Teneligliptin glucose dependently increases

*Corresponding author (Sohan S. Chitlange)

E-mail: < sohanchitlange@rediffmail.com > © 2017, Har Krishan Bhalla & Sons
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566
Fig. 1. Chemical structure of Teneligliptin hydrobromide hydrate
Downloaded by [University of New England] at 20:54 08 November 2017
insulin secretion and lowers glucagon secretion
thus resulting in an overall improvement in the glu-
cose homoeostasis3. Structure of teneligliptin
hydrobromide hydrate is shown in Fig. 1.
Literature survey revealed one reported method
by UV 4 and one by HPLC 5 for analysis of
Teneligliptin hydrobromide hydrate and no HPTLC
method reported for analysis of Teneligliptin
hydrobromide hydrate in bulk and pharmaceuti-
cal dosage form. Also teneligliptin in plasma has
been analysed and reported 6. The present work
describes a simple, precise, rapid, selective, and
economic high-performance thin-layer chromato-
graphic procedure and UV spectrophotometric
methods for determination of Teneligliptin
hydrobromide hydrate in bulk and tablet dosage
form. The proposed methods were optimized and
validated as per ICH guidelines 7-10.
High Performance Thin Layer Chromato-
graphic Method
Materials and methods
Teneligliptin hydrobromide hydrate pure drug
was gifted by Lupin limited, Aurangabad. Tablet
of teneligliptin Zita plus (20 mg of teneligliptin
hydrobromide hydrate, Mfg by:- Glenmark Phar-
maceuticals Pvt. Ltd., Solan HP), were purchased
from local market. All chemicals and reagents
used were of HPLC/AR grade.
Standard stock solution
12.5 mg of Teneligliptin hydrobromide hydrate
was accurately weighed and transferred to 25.0
ml volumetric flask, dissolved and diluted to the
mark with methanol (Concentration 500 μg/ml of
557
THH).
Selection and optimization of mobile phase
composition
2 μl of standard stock solution was applied on
TLC plates in the form of band (band size: 6 mm).
Different combination of solvent with varied po-
larity were tried to get well separated bands of
the drugs. After trying several permutations and
combinations, the solvent system containing tolu-
ene: methanol: triethylamine (8:2:0.2 v/v/v) was
found to be most satisfactory as it gave good sharp
peak with acceptable Rf value.
Selection of wavelength for densitometric
evaluation of separated bands
2 μl Standard stock solutions was applied on
TLC plate with the help of CAMAG LINOMAT-
V automatic sample applicator, the plate was
chromatographed in twin-through glass chamber
saturated with mobile phase for 10 minute. After
chromatographic development, the plate was re-
moved and air dried. The separated bands on the
TLC plate were scanned over the wavelength
range of 200-400 nm. From the spectra it was
observed that THH exhibit significant absorbance
at 254 nm which was selected for densitometric
evaluation of separated bands. Typical densitogram
of Teneligliptin is shown in Fig. 2.
Instrumentation and optimized chromato-
graphic conditions
Chromatographic analysis was performed on 10
cm × 10 cm aluminium backed plates coated with
0.2 mm layers of silica gel 60 F254 (E. Merck
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566
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Fig. 2. Densitogram showing Teneligliptin (Peak 2)
Germany). Samples were applied to the plates as
6 mm bands, 5 mm apart, under the continuous
flow of nitrogen using Camag Linomat V sample
applicator fitted with a 100 microlitre syringe
(Hamilton, Bonaduz, Switzerland). A constant
application rate of 150 nL s-1 was used. Linear
ascending development of the plates to a distance
of 80 mm was performed with toluene: methanol:
triethylamine (8:2:0.2 v/v/v) as mobile phase in a
twin-trough glass chamber previously saturated
with mobile phase vapour for 10 min at room tem-
perature (25°C). After chromatographic develop-
ment, the plate was air dried and scanned at 254
nm by means of a Camag TLC scanner III, con-
trolled by WINCAT’s software version 4, in re-
flectance-absorbance mode using the deuterium
lamp. The slit dimensions were 5 mm × 0.45 mm
and the scanning speed was 20 mm s-1. Concen-
trations of the compounds chromatographed were
determined from the intensity of the diffused light.
Calibration plot for Teneligliptin hydro-bro-
mide hydrate
12.5 mg of THH was accurately weighed and
transferred to 25.0 ml volumetric flask, dissolved
and diluted to the mark with methanol (Concen-
tration: 500 μg/ml).
The above solution was applied on the TLC plate
in the range 1-6 μl/band with the help of micro
syringe using LINOMAT V automatic sample
applicator. The plate was then developed and
scanned under the above mentioned chromato-
558
graphic conditions. Peak area was recorded for
each drug concentration and the calibration curves
of the concentration vs. peak area were con-
structed for teneligliptin.
Preparation of sample solution
Twenty tablets were weighed and crushed to
obtained fine powder. Average weight of tablets
was calculated. Accurately weighed quantity of
tablet powder equivalent to about 12.5 mg of THH
was transferred to 25.0 ml volumetric flask; 15
ml methanol was added and ultrasonicated for 15
min., volume was then made upto the mark with
methanol. The solution was mixed and filtered
through Whatmann filter paper No. 42. The fil-
trate was used as sample solution. Two bands of
standard stock solution and four bands of sample
solution, 4.0 μl each, were applied and developed
on TLC Plate and scanned under the optimum
chromatographic condition. After scanning the
peak obtained for standard and sample bands were
integrated. Amount of drug present in sample was
calculated by comparing the mean peak area of
sample band with that of the standard band.
Method validation
The method was validated in compliance with
ICH guidelines.
Accuracy
Tablet powder equivalent to about 12.5 mg THH
was accurately weighed and transferred individu-
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566
ally in nine different 25.0 ml volumetric flasks,
add 10 mg, 12.5 mg and 15 mg of THH pure drug
to the sample into three volumetric flasks for 80
%, 100 % and 120 % level of recovery, respec-
tively. All dilutions were performed with metha-
nol. Solutions were prepared in triplicate and
analysed. Accuracy was determined and ex-
pressed as percent recovery.
Precision
Precision studies were performed to ascertain
repeatability and reproducibility of the method.
Sample solution was prepared and analysed in the
Downloaded by [University of New England] at 20:54 08 November 2017
similar manner as described under analysis of the
marketed formulation. Intra-day precision was
determined by analyzing a sample solution at three
different time intervals on the same day and in-
ter-day precision was determined by analyzing a
sample solution on three consecutive days.
Limit of Detection (LOD) and Limit of
Quantitation (LOQ)
The LOD and LOQ were separately determined
based on the standard deviation of response of
the calibration curve. The standard deviation of
y-intercept and mean of slope of the calibration
curves were used to calculate the LOD and LOQ.
Robustness
Small but deliberate variations in the optimized
method parameters were done to evaluate the
robustness of the proposed method. By introduc-
ing small changes in the mobile phase composi-
tion, mobile phase volume, duration of chamber
saturation with mobile phase, time from spotting
to development (5 min, 20 min, 40 min and 1 hr)
and time from development to scanning (5 min,
20 min, 40 min and 1 hr), the effects on Rf value
and peak area of drug was examined. The com-
position of mobile phase was changed slightly (±
0.1 ml for component). TLC plates with standard
and sample bands were run with mobile phases
of composition toluene: methanol: triethylamine
(7.9:2.1:0.2 v/v/v and 8.1:1.9:0.2 v/v/v). Mobile
phase volume and duration of chamber saturation
were varied at 10.0 ml ± 1.0 ml (9, 10 and 11 ml)
and 10 min ± 20 % (8, 10 and 12 min), respec-
tively.
559
Forced degradation studies
In degradation studies, forced degradation was
tried by exposing a sample to following stress
conditions: acidic (2.0 M HCl), alkaline (0.05 M
NaOH), oxidation (3 % H2O2) and neutral hy-
drolysis using distilled water. For forced degrada-
tion contents of the flasks were refluxed with 3
ml of above solvents and 3 ml methanol in a wa-
ter bath at 80°C for 3 hr. For heat and photo deg-
radation a sample was kept at 60°C and in UV
light (254 nm) for 24 hr, respectively. After the
respective time intervals all the flasks were re-
moved and allowed to cool. The samples were
then analyzed in similar manner as described un-
der analysis of THH in formulation.
Result and discussion
Linearity
Peak areas were found to have good linear re-
lationship with the concentration than the peak
heights. Teneligliptin hydrobromide hydrate was
found to give linear detector response in the
concentration range of 0.5-3 μg/band (shown in
Fig. 3). The straight line equation and coefficient
of correlation for THH calibration curve was y =
2592.8x + 2611.7 and r² = 0.9993 respectively.
Analysis of marketed formulation
Analysis of marketed formulation containing
THH (20 mg) was carried out and results are ex-
pressed as percentage amount of the label claim.
The average weight of tablet was 362.775 mg.
There was no interference from the excipients.
The THH content was found to be close to 100
% and the result is summarized in Table 1. The
low SD value indicated the suitability of this
method for routine analysis.
Accuracy
To determine the accuracy of proposed method,
recovery studies were carried out by standard
addition method and the results are expressed as
percent recovery. The mean percentage recov-
ery for each compound was calculated at each
concentration level and reported with its standard
deviation. The percentage recovery at three lev-
els (80 %, 100 % and 120 %) was found to be
satisfactory (Table 2) indicating the accuracy of
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566 560
Downloaded by [University of New England] at 20:54 08 November 2017

Fig. 3. Calibration curve of Teneligliptin at 254 nm

Table 1. Results of analysis of marketed formulation

Brand name Label claim Amount estimated* % Label claim*± SD

(mg) (mg/tab)

Zita plus 20 20.053 100.266 ± 0.78

*mean of six observations

Table 2. Results of accuracy studies

% Level of Percent % RSD Mean %

recovery recovery*± SD recovery** ± SD

80 100.71±0.739 0.734 100.49± 0.76

100 99.99±1.306 1.307
120 99.41±1.262 1.27

*mean of three observations

**mean of nine observations
developed method.
Precision
Precision was evaluated by carrying out in-
dependent sample preparation of a single lot of
formulation on same day 3 times and on three
different days. Standard deviation and percent-
age relative standard deviation (% RSD) was
found to be less than 2 % for intraday and inter
day precision (Table 3) indicating the repeat-
ability and reproducibility of the developed
method.
Limit of detection (LOD) and limit of quanti-
tation (LOQ)
LOD and LOQ values for THH was found to
be 0.0935 and 0.2834 μg/band, respectively. The
low LOD and LOQ values for THH indicate the
sensitivity of the method.
Robustness
The robustness studies were done by observing
the effect of change in mobile phase composition
(± 0.1 ml), chamber saturation time (± 20 %), time
from application to development (5, 20, 40, 1 hr),
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566 561
Table 3. Results of precision studies

Precision % Label claim* ± SD % RSD

Intra-day precision 100.006 ± 0.453 0.453

Inter-day precision 100.72 ± 0.514 0.51

*mean of three observations

time from development to scanning (5, 20, 40, 1 hr)
on the Rf value of drug was studied. The method
was found to be unaffected by small changes in
method parameters with % RSD for Rf values un-
der varied method parameters less than 2.0 %. The
Downloaded by [University of New England] at 20:54 08 November 2017
methanol. The resulting solution was scanned in
the range of 200-400 nm to determine the wave-
length of maximum absorbance. Teneligliptin
hydrobromide hydrate has shown maximum ab-
sorption at 247 nm (shown in Fig. 7).

developed method is considered to be robust.

Forced degradation studies
Forced degradation of THH was tried under dif-
ferent stress conditions such as acid hydrolysis (2.0
M HCl), alkaline hydrolysis (0.05 M NaOH), oxi-
dation (3 % H2O2), neutral hydrolysis, heat and
exposure to UV radiations. Teneligliptin was found
to degrade more in alkaline and peroxide stress con-
ditions as compared to acidic conditions. The per-
cent assay of active substance and the Rf values
of degradation products are given in Table 4.
Densitogram of acid, alkaline and peroxide treated
samples are shown in Fig. 4, 5 and 6 respectively.
UV Spectrophotometric Method
Determination of wavelength of maximum ab-
sorption
The standard stock solution of 100 μg/ml of
teneligliptin hydrobromide hydrate was prepared
by weighing 10 mg of the drug, taken in 100 mL
volumetric flask and diluted with methanol. Take
4 ml of above solution and dilute it to 10 ml with
Table 4. Results of forced degradation study
Assay of Teneligliptin hydrobromide hydrate
tablet formulation
Twenty tablets were weighed and crushed to
obtain fine powder. Average weight of tablets
was calculated. Accurately weighed quantity of
tablet powder equivalent to about 10.0 mg of THH
was transferred to 100.0 ml volumetric flask, added
30 ml methanol and ultrasonicated for 10 min,
volume was then made upto the mark with metha-
nol. The solution was mixed and filtered through
Whatmann filter paper no. 42. Then 5.0 ml fil-
trate was diluted to 25.0 ml with methanol. Ab-
sorbance of resulting solution was measured at
247.0 nm. The concentration of THH in the
sample was calculated by using straight line equa-
tion of calibration curve. The % assay of the drug
was calculated.
Method validation
The proposed method was validated for differ-
ent parameters like linearity, precision, accuracy,
ruggedness, robustness, LOD, LOQ and assay.

Stress condition Percent assay of Rf value of

active substance degraded product

Acid (2.0 M HCl, 80ºC for 3 hrs) 89.038 0.07, 0.12, 0.44, 0.61
Alkali (0.05 M NaOH, 80ºC for 3 hrs) 70.252 0.13, 0.25, 0.47, 0.62
Oxide (3 % H2O2, 80ºC for 3 hrs) 75.034 0.06, 0.13, 0.35
Neutral (Distilled water, 80ºC for 3 hrs) 99.157 -
Heat (60ºC for 24 hrs) 98.741 -
UV-Exposure (254nm for 24 hrs) 99.885 -
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566 562
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Fig. 4. Densitogram of acid (2.0 M HCl) treated sample

Fig. 5. Densitogram of alkali (0.05 M NaOH) treated sample

Fig. 6. Densitogram of oxide (3% H2O2) treated sample

 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566
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Fig. 7. UV Spectra of Teneligliptin hydrobromide hydrate
Linearity study
The linearity was determined by plotting con-
centration against corresponding absorbance.
Standard stock solution, 100 μg/ml were further
diluted with methanol to obtain 5, 10, 20, 30, 40,
50 μg/ml solutions. The calibration curves were
constructed by plotting absorbance versus con-
centration and the coefficient of correlation and
straight line equation were calculated.
Intra-day precision study
Aliquot (2 ml) of the 100 μg/ml THH stock so-
lution was taken in 10 ml volumetric flask and
diluted with methanol to obtain 20 μg/ml. Tripli-
cate absorbance measurements were made for
three times on same day and the percentage RSD
was calculated.
Inter-day precision study
The selected concentration for the intra-day pre-
cision study was again analysed for three con-
secutive days and the percentage RSD was cal-
culated.
Recovery Studies
Accuracy of the method was calculated by re-
covery studies at three different levels (80 %, 100
% and 120 %) in triplicate at each level by stan-
dard addition method to study the accuracy of the
method and to check the interference from ex-
563
cipients. The percentage recovery in each case
was calculated.
Ruggedness
The ruggedness of an analytical method is the
degree of reproducibility of test results obtained
by the analysis of the same homogeneous samples
under a variety of conditions such as different
laboratories, different analysts, different instru-
ments, different lots of reagents, different elapsed
assay times, different assay temperatures, differ-
ent days, etc. Ruggedness is normally expressed
as the lack of influence of operational and envi-
ronmental factors of the analytical method. It was
determined by carrying out analysis on different
instruments and different analyst. The absorbance
and assay was carried out three times.
Robustness
The robustness of an analytical procedure is the
measure of its capacity to remain unaffected by
small but deliberate variations in method param-
eters and provides an indication of its reliability
during normal usage. It was determined by car-
rying out the analysis at λ max ± 1 nm. The ab-
sorbance and assay was carried out three times.
Limit of detection (LOD) and limit of quanti-
tation (LOQ)
The LOD and LOQ were separately determined
 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566
based on the standard deviation of response of
the calibration curve. The standard deviation of
y-intercept and mean of slope of the calibration
curves were used to calculate the LOD and LOQ.
Result and discussion
Linearity
Teneligliptin hydrobromide hydrate was found
to give linear detector response in the concentra-
tion range of 5-50 μg/ml (shown in Fig. 8). The
straight line equation and coefficient of correla-
tion for THH calibration curve was y = 0.0238x +
0.0148 and r² = 0.9997 respectively.
The result of analysis of marketed formulation
Downloaded by [University of New England] at 20:54 08 November 2017
564
hydrobromide hydrate can be determined in bulk
and in pharmaceutical formulation without inter-
ference from the excipients. The proposed
HPTLC method gave sharp peak for THH and
was also able to selectively quantitate THH in
presence of the degradation products obtained in
forced degradation study. Hence, the methods can
be employed as a stability indicating one. The UV
method proposed is also a good alternative for
analysis of THH. ICH guidelines were followed
throughout method validation and the suggested
method can be applied for routine quality control
analysis of pharmaceutical formulation contain-
ing the drug.

is shown in Table 5. The results of the validation

parameters of the proposed UV method are sum-
marized in Table 6, 7, 8, 9 and 10.
Conclusion
Based on the results obtained it is concluded
that both the methods are sensitive, accurate, pre-
cise and reproducible, where teneligliptin
Acknowledgement
The authors are thankful to Dr. P.D. Patil, Chair-
man, Dr. D.Y. Patil Vidya Prathisthan Society,
Pimpri, Pune for providing necessary facilities.
Authors are also thankful to Lupin limited,
Aurangabad, for providing gift sample of
teneligliptin hydrobromide hydrate pure drug.

Fig. 8. Calibration curve of THH at 247 nm

Table 5. Results of Accuracy

% Level of Percent % RSD Mean %

recovery recovery*± SD Recovery**± SD

80 98.968 ± 0.2 0.202 99.982 ±1.02

100 100.265 ± 0.549 0.547
120 99.982 ± 1.320 1.321

*mean of three observations; **mean of nine observations

 Sohan S. Chitlange et al., / TACL 7 (4) 2017 556 - 566 565
Table 6. Results of precision studies

Precision % Label claim* ± SD % RSD

Intra-day precision 99.58 ± 0.193 0.194

Inter-day precision 100.81 ± 0.581 0.584

*mean of three observations

Table 7. Results of LOD and LOQ

Limit of detection (μg/ml) 1.53

Limit of quantification (μg/ml) 4.65
Downloaded by [University of New England] at 20:54 08 November 2017

Table 8. Results of robustness studies

Robustness Label claim* ± SD % RSD

At 246 nm 99.131 ± 1.19 1.2

At 248 nm 99.271 ± 1.273 1.283

*mean of three observations

Table 9. Results of ruggedness studies

Ruggedness Instrument Analyst

1 2 1 2

% Label Claim** 99.415 99.134 99.57 99.08

S.D. (±) 1.12 1.17 1.10 0.58

Table 10. Results of analysis of marketed formulation

Brand name Label claim Amount estimated* % Label claim*

(mg) (mg/tab) ± SD

Zita plus 20 19.861 99.307 ± 1.04

*mean of six observations

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