A selective Ultra Performance Liquid Chromatographic (UPLC) method for the determination of Magnesium Valproate and its process related impurities has been developed. The method includes reversed-phase Acquity BEH C18 column with 100 mm × 2.1 mm i.d. and 1.7µ particle size. The mobile phase consists of acetonitrile and 5mM ammonium di-hydrogen orthophosphate with pH = 3.0 and acetonitrile at 45:55 isocratic elution. The flow rate was 0.3 ml/min and UV detection was performed at 215 nm. A System Suitability Test (SST) was developed to govern the quality of the separation. The developed method has been validated further with respect to linearity, accuracy, precision, selectivity, LOD, LOQ and robustness. Different batches of samples were examined using this method, the method proved to be successful when applied to analyze a commercial magnesium valproate formulation.
KEYWORDS
Magnesium Valproate,Ultra Performance Liquid Chromatography, Process Related Impurities, Method Validation, Isocratic Elution.
Magnesium Valproate is chemically known as Magnesium 2-propylpentanoate. Magnesium Valproate is an anticonvulsant used in the treatment of epilepsy and bipolar disorder, as well as other psychiatric conditions requiring the administration of a mood stabilizer.[1-6] Chemical structures of magnesium valproate and four of its process related impurities are given in Fig.01. To our knowledge, there is no paper describing an Ultra Performance Liquid Chromatographic (UPLC) method that allows the separation of magnesium valproate and its impurities in bulk drugs. Some articles exist on isocratic liquid chromatographic methods for the determination of magnesium valproate.[7, 8] However, these isocratic methods use short columns and are suitabl...
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...valproate and its related impurities were added to the samples and the recovery was calculated which was between the 98-102%, these were well within the acceptance criteria.
The method precision was assessed using multiple preparations of a single sample. Six different preparations of the same magnesium valproate and its related impurities sample, each 0.20 mg/ml, were analyzed in triplicate on the same day. New solutions were prepared and analyzed on each of two successive days. The % RSD values obtained for the peak areas of magnesium valproate, velaronitrile, pentanoic acid, 2-ethyl pentanoic acid and 2-(1-methyl, ethyl) pentanoic acid were not more than 2.0. The intermediate precision study was performed using another Acqity BEH C18 column (100 mm × 2.1 mm i.d., 1.7μ particle size) and by different analyst. The % RSD values were of the same magnitude as above.
This excessive yield was resultant of the impurities within the product, where the solvents, particularly the dichloromethane, were not sufficiently removed from the product. In figure 3, the peak at 5.22 ppm with a normalised intensity of 1.00 evidenced the significant proportion of the dichloromethane in the product, and the peak at 0.88 ppm with a normalised intensity of 0.25 indicated some remaining hexane.4 The unreasonable yield was mostly attributed to these.
For this solution, 5 mL of the solution with 2.5 mL of AMV was placed in the cuvette. The cuvette was placed inside of spectrophotometer and the amount of absorbance was recorded. This procedure that involves a solution with a known concentration was repeated for the concentrations:1.0x10-4 M,5.0x10-5 M,2.0x10-5M, and1.0x10-5M.A unknown solution absorbance was measured by putting 5 mL of unknown solution with 2.5 mL AMV in a cuvette. The cuvette was placed in the spectrophotometer and the amount of absorbance was recorded. The procedure that deals with the unknown solution was repeated 2 more times with the same solution and the same amount of solution and AMV.
Firstly, an amount of 40.90 g of NaCl was weighed using electronic balance (Adventurer™, Ohaus) and later was placed in a 500 ml beaker. Then, 6.05 g of Tris base, followed by 10.00 g of CTAB and 3.70 g of EDTA were added into the beaker. After that, 400 ml of sterilized distilled water, sdH2O was poured into the beaker to dissolve the substances. Then, the solution was stirred using the magnetic stirrer until the solution become crystal clear for about 3 hours on a hotplate stirrer (Lab Tech® LMS-1003). After the solution become clear, it was cool down to room temperature. Later, the solution was poured into 500 ml sterilized bottle. The bottle then was fully wrapped with aluminium foil to avoid from light. Next, 1 mL of 2-mercaptoethanol-β-mercapto was added into fully covered bottle. Lastly, the volume of the solution in the bottle was added with sdH2O until it reaches 500 ml. The bottle was labelled accordingly and was stored on chemical working bench.
The objective of this experiment was to perform extraction. This is a separation and purification technique, based on different solubility of compounds in immiscible solvent mixtures. Extraction is conducted by shaking the solution with the solvent, until two layers are formed. One layer can then be separated from the other. If the separation does not happen in one try, multiple attempts may be needed.
Also, it had provided enough trials to find an accurate volume of Ca(OH)₂. The data collected gave enough information to find the mol of H⁺ ions which equaled the mol of OH⁻ ions because of neutralization. Furthermore, this helped to find the concentration of OH⁻, which helped find the concentration of Ca²⁺ because every 2 OH⁻ ions have one Ca²⁺ ion. That is why the concentration of Ca²⁺ was half of the concentration of OH⁻. With these two concentrations the Ksp was found which was 2.92 x 10^⁻⁵. The actual Ksp is 5.5 x 10^⁻⁶, therefore, there is a big difference. In fact, the percentage error is 431%. This could of happened because of some sources of errors in the
Size and stability: Liquid formulation can be bulky, difficult to transport and store.1 During storage under the stated conditions, it’s necessary that oral solutions are not subject to precipitation, fast sedimentation, caking or formation of lump.2 They have poor stability compare to solid dosage form formulation due to hydrolysis.1 Therefore, it’s important to optimize the active ingredient stability in liquid formulation including those prepared from powder or granules.2
Once the mixture had been completely dissolved, the solution was transferred to a separatory funnel. The solution was then extracted twice using 5.0 mL of 1 M
During week 1 of this experiment, we recorded common components of fertilizers and then went on to find the chemical formulas involved in creating them. The second week we began the process of comparing three authentic ions we had established in the first week to ion samples to discover other properties they might contain. We decided to discover these different ingredients by preforming a serious of tests, which included placing 0.2g solid of both the authentic and the sample fertilizer separately, in order to establish a constant, and dissolved the fertilizer in 20 mL of water, then checked to see if Mg was present in the sample solution. By setting up a constant and preforming a methodical experiment all on the samples given, we demonstrated the ability to correctly establish and preform an experiment and solve the problem at hand, which was distinguishing the contents of the authentic
..., and is immiscible with water. Since there was not clear distinct two layers after steam distillation, extraction was used to separate the eugenol from water thus, steam distillation is not an effective way to isolate eugenol by itself. In order to determine how pure the isolated eugenol was, TLC was performed and compared to the standard and 1H NMR of the isolated eugenol and standard were compared to conclude that the extracted compound was eugenol with some impurities.
A condenser and heat reflux was used to prevent reagents from escaping. Then the solid product was vacuum filtered. The product was recrystallized to purify it and the unknown
Analysis of Aspirin Tablets Aim --- To discover the percentage of acetylsalicylic acid in a sample of aspirin tablets. ----------------------------------------------------------------- In order to do this, the amount of moles that react with the sodium hydroxide must be known. This is achieved by using the method of back titration.
Furthermore, an additional method to use other hydrochloric acids that have different concentration levels such as 1 M and 2.5 M ones, can improve the outcome of the results. This increases the variation of the independent variable, which accordingly increases the precision of results.
Aim: The aim of this experiment was to determine the empirical formula of magnesium oxide.
Gusdinar T. COMPLEXOMETRIC TITRATION An application method of Inorganic Pharmaceutical Analysis [homepage on the internet] . No date. [cited 2014 Mar 20]. Available from: http://download.fa.itb.ac.id/filenya/Handout%20Kuliah/Inorganic%20Pharmaceutical%20Analysis%202008/English%20Version/05.%20COMPLEXOMETRIC%20TITRATION.pdf.
Materials and Methods: An ion exchange chromatography column was obtained and set up for purification with the addition of 0.5 ml ion exchange matrix. 1 ml