Determination of Pravastatin Sodium Using Atomic Absorption Spectrometry Based on its Sodium Content
Nasr M. El-Abasawi, Khalid A.M.
Attia, Ahmad A. M. Abo-Serie, Samer Morshedy, Ashraf Abdel-Fattah*
Pharmaceutical Analytical Chemistry
Department, Faculty of Pharmacy, Al-Azhar University, Nasr City, Cairo, Egypt
*Corresponding author: Ashraf Abdel-Fattah, Pharmaceutical Analytical
Chemistry Department, Faculty of Pharmacy, Al-Azhar University, 11751 Nasr
City, Cairo, Egypt. Tel: +201009408060; Email: ashraf.abdelfattah@hotmail.com
Received Date: 30 June, 2018; Accepted Date: 03 August,
2018; Published Date: 10 August, 2018
Citation: El-Abasawi NM, Attia KAM, Abo-Serie AAM, Morshedy S, Abdel-Fattah A (2018) Determination of Pravastatin Sodium Using Atomic Absorption Spectrometry Based on its Sodium Content. Arch Anal Bioanal Sep Tech: AABST-107. DOI: 10.29011/AABST-107. 100007
1. Abstract
Atomic spectroscopy is one of the most widely used methods for quantitative elemental analysis. An atomic absorption spectrometric method was developed and validated as a direct, simple and sensitive method for determination of pravastatin sodium which, based on its sodium content at 589 nm without tedious or complex procedures. The developed method is very sensitive regarding LOD (0.026 ppm of sodium equivalent to 0.479 µg/ml), LOQ (0.079 ppm of sodium equivalent to 1.454 µg/mL) with a linear range of (0.2 - 1.0 ppm equivalent to 3.37 - 16.84 µg/ml). The proposed method was validated according to International Conference on Harmonization (ICH) guidelines and successfully applied for the determination of pravastatin sodium in its dosage form.
2. Keywords: Pravastatin Sodium; Absorption Spectrometry; Elemental Analysis; Selective Determination
3.
Introduction
Pravastatin sodium
is sodium
(3R,5R)-7-{(1S,2S,6S,8S,8aR)-1,2,6,7,8,8a-hexahydro-6-hydroxy-2-methyl-8-[(S)-2-methylbutyryloxy]-1-naphthyl}-3,5-dihydroxyheptanoate
[1-2]. It is a selective and competitive
inhibitor of 3-hydroxy-3- methylglutaryl -coenzyme A (HMG-CoA) reductase. Atomic Absorption
Spectroscopy (AAS) is a spectroanalytical procedure for the quantitative
determination of chemical elements using the absorption of optical radiation
(light) by the free atoms in the gaseous state. It is generally acknowledged
that if sufficient analyte is present in the sample, then it should be
determined using a flame technique because this has added advantages of being
rapid (assuming only a few elements need be determined) and, in comparison with
alternative techniques, very simple to use. AAS can be used to determine over
70 different elements in solution, or directly in solid samples via
electrothermal vaporization. Reviewing the
literature on the determination of pravastatin in pharmaceutical dosage forms
and/or biological fluids, including HPLC methods for the determination of
pravastatin are reported [3-6], LC [7-9], Spectrophotometric methods [10-15], electrochemical methods [16], electrophoresis [17]. The
main goals of analytical atomic spectrometry are to attain the lowest limits of
detection (down to single atoms), use the broadest dynamic range, suppress the
matrix effect, eliminate spectral interferences, minimize the time and cost
required for sample preparation [18]. Reviewing
the literature on the pravastatin sodium in its commercial dosage form, reveals
that there is no atomic spectrometric method was applied for determination of
pravastatin sodium. The main aim of this work is to develop a simple, sensitive
and inexpensive atomic absorption spectrometry method for the determination of
pravastatin-sodium in its pure and dosage forms through estimation of its
sodium content.
4.
Experimental
4.1
Materials
4.1.1
Pure Samples: Pure pravastatin (99.52%) was kindly supplied by kindly
supplied by National Organization for Drug Control and Research, Giza, Egypt.
4.1.2
Pharmaceutical
preparation: Lipostat® tablets labeled to contain 40 mg of
pravastatin per tablet (B.No. N109338), manufactured by SmithKline Beecham,
Egypt Cholestate® tablets labeled to
contain 10 mg of pravastatin per tablet (B.No. HP0013), manufactured by
Hi-Pharm, Egypt.
4.1.3
Chemicals and
Reagents: Water used throughout the procedure
was freshly double distilled.
4.1.4
Apparatus: A thermo elemental
atomic absorption flame spectrophotometer, (Cambridge - UK) serial no. JE710572
computed with solar data station software version 9.03. Sodium was measured at
wavelength 589 nm, band pass 0.5 nm, relative noise 1.0 nm, lamp current 10 mA,
integration time 5 second.
4.1.5
Standard Solutions
A stock solution of the pravastatin
(0.1mg/ml) was prepared by dissolving 10 mg of pravastatin-sodium in 50 ml
double distilled water and the volume was completed to 100 ml with the same
solvent.
4.2
Procedures
4.2.1
General Procedure
Aliquots
of the standard
pravastatin-sodium solution
(0.1mg/ml) containing
(36.8-184.2μg) m of the drug equivalent to (2-10 ppm Na) were transferred into a series of 10-ml volumetric flasks, completed to the mark with double
distilled water. The drug was determined
through its sodium content at 589 nm.
4.2.2
Procedure for
Pharmaceutical Preparation
Ten tablets of Lipostat® and Cholestate® tablets labelled to contain
40 mg and 10 mg of pravastatin-sodium per tablet respectively were weighed, finely powdered and mixed carefully. An accurately
weighed quantity of the powder equivalent to 10 mg of pravastatin sodium was
introduced into a 100-mL volumetric flask, extracted with 50 ml double
distilled water by shaking for 5 minutes. The volume was completed to the mark
with the same solvent and then filtered to obtain a solution labeled to contain
(0.1 mg/ml) to be analyzed by the proposed method. The drug concentrations were
calculated from the corresponding regression equation.
4.2.3
Reported Method [19]
Pravastatin and pioglitazone were
determined simultaneously using the first derivative method at 249.7 and 277 nm
for pravastatin and pioglitazone, respectively. This method was applied on
Pravazon® capsules which contain 10
mg of each drug per capsule.
5.
Results and Discussions
5.1
In the Present Study: A simple and
sensitive Atomic Absorption Spectrometry (AAS) procedure was suggested for
quantitative determination of pravastatin-sodium through its sodium content at λs589 nm.
5.2
Method Validation [20-21]
· Linearity and Range
Under the described experimental
conditions, the calibration graph for the method was constructed by plotting
the absorbance values versus drug concentrations in µg/ml. The regression plot
was found to be linear over the range of (36.8-184.2 μg/ml)
of pravastatin-sodium equivalent to (0.2-1 ppm) of sodium; as shown in figure 1. Linearity range, regression
equation, intercept, slope and the determination coefficient for the
calibration data were presented in Table 1.
·
Limits of
Detection and Quantitation
LOD and LOQ values
were calculated according to ICH guidelines [20] from the following
equations:
LOD = 3.3 σ / S
LOQ = 10 σ/ S
Where σ is the residual standard deviation of regression
lines and S is the slope of the calibration curve.
LOD and LOQ
values were calculated for the proposed procedures and the obtained results
indicated the sensitivity of the proposed method as shown in Table 1.
· Accuracy and Precision
The values of %
Recovery confirm excellent accuracy. Moreover, the small values of %RSD indicate the high precision of the method, as shown in Table 1.
· Specificity
The standard addition technique was
applied to check the specificity of the described method by adding aliquots of
the studied drug in its pure form (equal to 0.2, 0.4 and 0.6 ppm of sodium) to
already analyzed pharmaceutical preparation (aliquots equivalent to 0.2, 0.4
and 0.6 ppm of sodium) and the percent recovery of the pure added was
calculated. The data listed in Table 2 indicate no matrix interference.
5.3
Pharmaceutical Applications
The proposed method was applied for the
selective determination of pravastatin-sodium in Lipostat® tablet. Satisfactory results were obtained
in good agreement with the label claim. The obtained results were statistically
compared to those obtained by the reported method [19].
No significant differences were found by applying t-test and F-test at 95%
confidence level [22] indicating good accuracy
and precision of the proposed method for the analysis of the studied drug in
its pharmaceutical dosage form, as shown in Table 3.
6.
Conclusion
Atomic absorption spectroscopy method was
successfully applied for determination of pravastatin sodium. This method has
the advantages of being sensitive and selective without any interference as it
selectively determines the metal (sodium) content in the samples to be
analyzed. The application of the proposed method on the different brands was
done was recovery 0f 101.25 and 101.45 for pravastatin in Lipostat® and Cholestate®,
respectively.
Figure 1: Calibration graph of pravastatin sodium by the proposed atomic absorption
spectrometry method.
Parameters |
Atomic absorption spectrometry |
|
Wavelength (nm) |
589 |
|
Linearity range |
ppm |
0.2 - 1.0 |
(μg/mL) |
3.37-16.84 |
|
- Regression Equation - Slope (b) - Intercept (a) |
Y*= bx**+ a |
|
0.4537 0.0153 |
||
Determination coefficient (r2) |
0.9996 |
|
Accuracy (%Recovery) |
101.52 |
|
Precision (%RSD)*** |
Repeatability |
1.371 |
Intermediate precision |
1.541 |
|
LOD |
ppm |
0.026 |
(μg/ml) |
0.479 |
|
LOQ |
ppm |
0.079 |
(μg/ml) |
1.454 |
|
Y* Absorbance of sodium at 589 nm. x**Pravastatinconcentration in (ppm). ***Values for 3 determinations of 3 different concentrations. |
Table 1: Regression and validation data for determination of pravastatin-sodium by the proposed atomic absorption spectrometry method.
Pharmaceutical (ppm) |
Pure (ppm) |
%Recovery |
|||||
Lipostat® |
|||||||
Taken |
Found* |
Added |
Found |
||||
0.2 |
0.2025 * |
0.2 |
0.2021 |
101.05 |
|||
0.4 |
0.4028 |
100.7 |
|||||
0.6 |
0.6029 |
100.48 |
|||||
Mean±%RSD |
100.74±0.284 |
||||||
Cholestate® |
|||||||
0.2 |
0.2029* |
0.2 |
0.2023 |
101.15 |
|||
0.4 |
0.4037 |
100.93 |
|||||
0.6 |
0.6021 |
100.35 |
|||||
|
100.81 ±0.409 |
||||||
* Average of five determinations. |
Table 2: Recovery study of pravastatin-sodium by adopting the standard addition technique via the proposed Atomic absorption spectrometry method.
Parameters |
Atomic absorption spectrometry |
Reported method [6] |
n* |
5 |
5 |
Average (% Recovery) |
101.25 |
100.07 |
%RSD |
1.307 |
0.564 |
Student’s t-test (2.306)** |
0.584 |
—— |
F value (6.388)** |
1.758 |
—— |
* Number of measurements ** The values in parenthesis are tabulated values of “t” and “F” at (P = 0.05). |
Table 3: Determination of pravastatin-sodium in Lipostat® tablet by the proposed atomic absorption spectrometry and reported methods.