Chemical Engineering and Science, 2013, Vol. 1, No. 1, 1-6
Available online at http://pubs.sciepub.com/ces1/1/1
© Science and Education Publishing
DOI:10.12691/ces-1-1-1
Quantitative Determination of Milnacipran by Simple
Colorimetric Methods
Md. Mubarakunnisa
1
, Avula Prameela Rani
1
, Seelam Harika
1
, Chandra Bala Sekaran
2,*
1
University College of Pharmaceutical Sciences, Acharya Nagarjuna University, Nagarjuna Nagar, India
2
Department of Biotechnology, Jagarlamudi Kuppuswamy Choudary College, Guntur, India
*Corresponding author: balumphil@gmail.com
Received December 23, 2012; Revised January 22, 2013; Accepted February 28, 2013
Abstract In the present study, two sensitive, precise and accurate spectrophotometric methods have been
developed for the determination of milnacipran in bulk and capsule formulation. The first method is based on the
reaction of milnacipran with ninhydrin in N,N'-dimethylformamide medium at 80°C temperature to form a colored
Ruhemann's purple, which exhibits absorption maximum at 575nm. The second method is based on extraction of
milnacipran into chloroform as ion-pair with bromothymol blue. The yellow colored ion-pair complex exhibits
absorption maximu m at 410n m. Beer’s law is obeyed in th e concentration ranges 2.5-37.5ȝg/mL and 2-12ȝg/ mL of
milnacipran for methods I and II, respectively. The effect of experimental variables were investigated and optimized.
The validation parameters like linearity, sensitivity, accuracy, precision and robustness were checked by following
the ICH guidelines. The proposed methods were applied for the analysis of milnacipran in capsule formulation with
good results.
Keywords: milnacipran, ninhydrin, bromothymol blue, Ruhemann's purple, ion-pair complex
1. Introduction
Milnacipran (MCN) or 1R 2S)-2 aminomethyl-N-N-
dimethyl-1-phenyl cyclopropane carboxamine ( Figure 1)
is an antidepressant, effective in the treatment of
fibromyalgia. MCN acts by inhibiting the reuptake of
serotonin and nor epinephrine neurotransmitters in 1:3
ratio [1,2,3] .
Figure 1. Structure of Milnacipran
The analytical methods reported for the determination
of MCN are based on chromatographic techniques. They
include RP-HPLC [4,5,6], LC-MS [7] , U-HPLC [8] and
HPTLC [9] . Most of the reported chromatographic
methods have tedious extraction procedures, time-
consuming, complex, multiple sample preparation steps,
expensive and requires a skilled person to operate the
instrument. Hence these methods are not suitable for
routine analysis of MCN in quality control and quality
assurance laboratories. Compared with the above
mentioned chromatographic methods, spectrophotometry
is considered as the most convenient analytical technique
in many of the quality control and quality assurance
laboratories because of its advantages, such as good
selectivity, less expensive, simple instrumentation and less
time consuming.
To the best of our knowledge, there are only few
reports on the determination of MCN using
spectrophotometric method [10,11,12,13]. These methods
have drawbacks such as insensitivity, lack of selectivity,
use of expensive reagent and rigid control of pH. In the
present paper, we report two spectrophotometric methods
for the estimation of MCN in bulk and capsules by using
ninhydrin and bromothymol blue as analytical reagents.
2. Materials and Methods
2.1. Apparatus
The absorption spectra and measurements were
recorded using a systronics (Schimadzu Corporation,
Tokyo, Japan), model visiscan-167, digital
spectrophotometer with 1-c m matched quartz cells.
Samples were weighed using a schimadzu electronic
weighing balance (Schimadzu Corporation, Tokyo, Japan)
BL 220H model.
2.2. Chemicals and Reagents
All reagents and chemicals were of analytical reagent
grade
1. Milnacipran was kindly provided by Matrix
laboratories (Hyderabad, India).
2. Milza capsules (Intas pharmaceuticals, Dehradun,
India), labeled to contain 50 mg milnacipran/capsule, were
purchased from hetero pharmacy (Guntur, India).