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Revue Roumaine de Chimie 2017, 62(2), 173-179
http://web.icf.ro/rrch/
capacity and low sample processing before quality acquired from Merck & Co, USA. High purity water
injection into the system. In recent times, there is a was obtained by using a Waters Milli-Q plus distillation
system.
direction to get economical, rapid and green
analysis method; FIA techniques fulfill this need in 2. Instruments
comparison with manual not automatic techniques.
Spectrophotometric estimation was operated on double
Furthermore, in recent years FIA has widespread beam UV-VIS Spectrophotometer Shimadzu 240 version 2.21
utilization as they can also be optimized rapidly for utilizing 10 mm quartz cells with 2 nm slit-width.
the compound analysis in comparison with the Polarographic system was Polaropulse Model BAS100B
conventional chromatographic methods.12,13 with controlled growth mercury electrode as the working
electrode and platinum wire was used as auxiliary electrode
Spectrophotometric techniques were developed
and saturated Ag/AgCl was used as a reference electrode. All
for the determination of MLS in dosage forms14,15 quantification was done at room temperature 25 ± 2 °C. A
and in combination with other drugs such as pure nitrogen gas 99.999% was used for deoxygenating.
Desloratadine16. Several other analytical techniques The FIA study was carried out by a Shimadzu (Kyoto,
such as spectrofluorimetric,17 high performance Japan) HPLC system constructed from the LC-20AT pump
and a model SPD-20A UV-VIS detector with manual injection
liquid chromatographic (HPLC) methods18 were also of standard solutions and samples. Various instrumental and
reported for its determination in human plasma. analytical parameters were examined for each methodology.
HPLC and derivative spectrophotometric method for
determination of MLS and loratadine in combined 3. Standard and sample preparation
tablet was found19. Assay of MLS in human serum The preparation of a stock solution of MLS 163.59 g/mL
specimen and MLS tablets on nickel hydroxide was done by dissolving the standard in 50% methanol then the
nanopetals modified carbon electrode,20 adsorptive working solutions were prepared by further dilution with the
stripping voltammetry of MLS in trade tablets and same solvent. To protect the solution form degradation by
light they were kept in an amber volumetric flask and all
biological specimen (urine and plasma) using experiments were carried out in darkness. The chemical
HMDE21 as well as direct current (DCt), differential stability of MLS was studied by a voltammetric method for a
pulse polarography (DPP) and alternating current period of 5 days; the reference solution was stored at 2–8°C in
(ACt) polarography for determination of MLS in a refrigerator. The voltammetric examination showed a peak
signal on the first day only which indicate that the solution is
dosage form and plasma22 were developed. The stable for 1 day for this reason working solution were prepared
superiority of the current developed OSWV method freshly every day.
over the already found electroanalytical methods are The method was applied to an MLS tablet according to the
no need for special electrode, necessity to accumulate United States pharmacopeia rules.23 For the analysis, 10
the drug on electrode surface which requires time tablets were weighed and pulverized. An amount of the
powder proportional to 10.0 mg of MLS was weighed
before detection, highly qualified analyst. In addition, precisely and transferred into a 100 mL volumetric flask. After
the detection limit of the OSWV developed method addition of a portion of 50% methanol the mixture sonicated
is considered satisfactory for the determination of for 30 min, then the volume of the solution was completed to
MLS in dosage forms. the 100 mL with the same solvent. For UV and FIA methods
the aliquots containing MLS were transferred into centrifuge
Overview of the literature showed that there is no tubes, the solution was centrifuged for 10 min at 20 °C at the
article for evaluation of MLS in tablet dosage form speed of 4000 rpm and then filter of 0.45 µm was used for
neither by FIA nor by OSWV is present till now. The filtration of working solutions. In case of OSWV analysis the
main aim of this study is to cope with the demands of solution examined without centrifuge or filtration. The
pharmaceutical analysis field for reasonable, high- regression equation calculated from the calibration graph of
the standard solution was used to calculate the nominal
throughput, immediate and sensitive determination of content of the tablets.
MLS in tablet dosage. The UV method was also
developed and recommended for the comparison of
OSWV and FIA. These methods would allow RESULTS AND DISCUSSION
determination MLS for routine analysis and quality
control in different laboratories equipped with
different analytical instruments. 1. Ultraviolet Spectrometry
Blank
Table 1
Regression data of the calibration curve for quantitative determination of MLS
Analytical Methods
Parameters Voltammetry FIA UV Spectrometry
Measured potential (V)
and Measured wavelength (nm) 0.6-0.8 344.4 344.4
Linearity Range (µg/mL) 3-16.5 3-16.5 3-16.5
Slope 6.79x10-9 34501 0.0429
Intercept 4.75x10-8 15189 0.0167
Regression 0.9976 0.9997 0.9989
SD of slope 1.29x10-10 514.3 0.00099
SD of intercept 1.4x10-9 5587 0.0108
LOD, µg/mL 1.142 0.8881 0.6384
LOQ, µg/mL 3.461 2.691 1.935
Within-day precision (RSD), % 1.788 1.679 1.288
Between-days precision (RSD), % 1.986 1.848 1.467
Max. 97.96% Max.100.08% Max. 101.45%
Accuracy recovery % Med.100.82% Med.100.24% Med. 99.55%
Low. 98.02% Low. 98.86% Low. 101.52%
SD:Standard Deviation, LOD:Limit of Detection, LOQ:Limit of Quantification, RSD: Relative Standard Deviation
MLS solutions of 3.27µg/mL, 9.8µg/mL, and determination can be performed without any
16.5µg/mL were used for accuracy studies. The separation step because the peak obtained from the
examination of intraday and interday accuracy of dosage form was similar to those obtained from the
the three methods was performed for three MLS standard with no interference from tablet
subsequent days.26 The accuracy results are highly excipients. Both OSWV and UV analysis are
acceptable for the determination of MLS since the convenient and accurate to be applied in
recoveries percent were almost close to 100% for laboratories lacking liquid chromatographic
both drug standard and product. instruments. The uniformity of the mobile solvent
To examine the repeatability of the method in the FIA makes the method considerable in
(Intraday) and intermediate precision (Interday), comparison with the customary chromatographic
medium concentration 9.8 µg/mL of the MLS methods. A slight superiority of FIA over the other
standard solution was examined for three days, six two methods was seen since, it is suitable for
times in a day. Good correlations were obtained for processing numerous samples on a daily basis due
both intra and interday’s experiments indicating to short analysis time, large sample capacity and
that the developed methods are highly precise and low solvent consumption especially in quality
analytically acceptable. The calculated relative control laboratories. To prove the developed
standard deviation (RSD) value is lower than 2% methods applicability the replicate analysis of
deviation from the nominal value of precision.27 pharmaceutical dosage form was performed and
The validation data are given in Table 1. the results were evaluated and validated
statistically in the Table 2.
6. Comparison of the Determination Methods Statistical comparison of the developed
methods was performed at the 95 % confidence
On the basis of the results in Table 1, the three level with the assist of Student’s t and F-Tests. The
methods can be accepted as an analytical technique obtained results from the analysis of MLS in tablet
for analysis of MLS in tablet dosage form. By dosage form by OSWV and FIA are in good
comparing the precision and accuracy of three agreement with those obtained by the UV methods
methods, all of the three methods are adequate which is used as a reference method. On the basis
from an analytical perspective. From the point of of results shown in Table 2, there was no
detection limit, UV analysis showed some considerable variation between the performances
superiority so it can be applied for the of the three methods since the corresponding
determination of low concentration samples with theoretical values for Student’s t and F-Test were
no need for derivatization steps. In the OSWV lower than the calculated values.28
Multiple analytical methodologies 179
Table 2
The results for the determination of MLS of dosage form
Labeled claim, mg 10 10 10