Chromatographic and Hyphenated Methods - Research Paper Example

 Chromatographic and Hyphenated Methods Nexium (esomeprazole magnesium) analysis Esomeprazole magnesium is a chemical substance that prevents gastric acid secretion. Its molecular structure is Its chemical formula is Magnesium 5-methoxy-2-[(4-methoxy-3, 5-dimethylpyridin-2-yl)methylsulfinyl]benzimidazol-1-ide Procedure 1- Planning the analysis Process Transfer contents 0.1 into1.0 mL volumes of standard solution containing esomeprazole magnesium to several conical standard flasks. Follow through with 2.2Ml containing 10-2 bromosuccinimide MN and warm the mixture at 35-1-C for about 12 minutes. Allow them to cool at room temperature of (25-1-C) (Holler, et al., 2006). Transfer the contents of the flasks to 5 volumetric standard flasks. Dilute the content with acetone up to mark. The absorbance should be 380nm against the reagent, which is blank and prepared simultaneously to omit esomeprazole magnesium. The colored substance will be stable for about an hour. Calculate the drug concentration through a regression corresponding equation or a calibration curve. Errors Several errors can occur in the process of making esomeprazole magnesium drug. First, the regents can be taken in large quantities or less quantities, which will affect the general outcome. Measuring cylinders must be used to avoid this error. Another error can arise during heating. This can either be lower than the required temperature therefore affecting the result. Thermometers should be available to take correct reading during the heating process. One can easily forget to transfer the reagents to 5 volumetric standard flasks. This will limit dilution of the reagents with the correct amount of acetone (Holler, et al., 2006). Following the right procedure and collecting all the requirements before the experiment will be helpful. Procedure 2- Identification - Qualitative Analysis of your active ingredient Components to assay During the experiment, the following components must be evaluated in the experiment. The quantity of esomeprazole in the product, which is the drug is one of the components to be determined. It is also significant to determine the stability of the drug in the environment. The process of preparing the drug should also be examined to ascertain its validity to the process (Holler, et al., 2006). Microanalysis During microanalysis, it is important to take keen interest in the following; the content of esomeprazole in the drug, functionality of the drug and the effects of the drug patients. It is also important to examine suitability of the drug to its function. The following should also be looked into Nexpro, torent, Raciper, ranbaxy, ezos ,Glenmark. Percentage ratio analysis of the ingredients The table below indicates the percentage ratios of all ingredients used in making esomeprazole medicine. Formulation Taken Added Found+_Sd2 Recovery % RSD2 CL Nexpro 20 30 30 99.9 0.106 0.079 Torrent 20 30 60 100 0.077 0.86 Raciper 20 30 30 99.98 0.093 0.069 Ranbaxy 20 30 60 99.99 0.099 0.088 Esoz 20 30 30 99.99 0.099 0.074 Glenmark 20 30 60 100 0.078 0.087 Separating active and inactive ingredients There are different methods for separating ingredients. One of the processes is base-acid extraction. This is a desirable method for separating valuable chemicals from the unwanted gunk. The principle behind this theory is that chemicals alkaloids in general, exist in two forms. Water-soluble component together with an acid and an oil, which is soluble freebase. A good example for this is pseudoephedrine or in other words Sudafed, which is a decongestant. This component is normally supplied in the form of a hydrochloride salt (HCL of pseudoephedrine). It is capable of existing inform of a base without a molecule of an acid. Therefore, it gets it’s free-base name from this perspective. It is possible to convert alkaloids from acid salts into free-bases. The same process can be reversed back to alkaloids by the use of a base or an acid (Ellis &Roberts, 2007). The practical part of it is that the chemical is chunked to increase the pH using a base like sodium hydroxide up to when the chemicals changes to a free base form to precipitate out. This is possible since the resultant solid is not soluble in water. At this point, anon-popular solvent is added, a layer of oil, for dissolving the chemical. After this, take time to shake properly the resultant feature is a non-popular layer that is required in search experiment. Dispose of the polar (water), the remainder shall be the non-polar layer which will be full of the required chemical. The same process can be reversed to get back the acid-base by adding an acid until when the freebase changes to an acid salt then precipitates out of the layer of non-polar component and throw away the layer of non-polar. This process is used to extract active ingredients from plant materials (Ellis &Roberts, 2007). An exemption is THC found in marijuana. It is not an alkaloid therefore; the process cannot help in extracting it. Procedure 3 - Quantitative analysis of your active ingredient Wet chemical analysis Wet chemical analysis is a method that excludes the use of instruments in the analysis of a chemical substance. Some of the methods in wet chemical analysis are gravimetry and titrimetry. They are mainly used for in the determination of quantitative properties of a sample. These methods can still be applicable in the analysis of the sample. Gravimetric analysis is a classical method in which a chemical substance is added to a known compound with an aim of forming a precipitate. The precipitate is then separate and weighed (Holler, et al., 2006). Volumetric analysis also referred to as titrimetry is where an unknown volume of a component is reacted with a known volume of another compound. With the help of reaction ratios, the volume of the unknown compound is determined (Holler, et al., 2006). Spectroscopic analysis The quantitative analysis of the chemical component of the sample will be carried out through a simple but sensitive spectrophotometric method. The sample of esomeprazole magnesium has maximum absorbance at 279 nm and follows the beer’s law at a concentration of between 4-40 micrograms/ml. Method Standard stock solution for the analysis will be made by dissolving around 40 micrograms of the sample in 100ml methanol. Various aliquots will then be fetched from the stock solution and diluted with a similar solvent to make a sequence of concentrations and then the calibration curve will be drawn. The solutions will then be analysed on a spectrophotometer in the UV range specified and their absorbances will be noted at around 279 nm while methanol AR grade will be applied as the blank (Ellis &Roberts, 2007). This method will be effective in the analysis of the substance because the parameters used are accurate, precise and robust. Accuracy will be assessed through a comparison with other intraday and inerday studies (Ellis &Roberts, 2007). Parameters such as Absorption maxima, Beer’s law, correlation coefficient, regression equation and slope will be the concepts of a spectroscopic method which would be applicable for the quantitative analysis of your active ingredient (Ellis &Roberts, 2007). Chromophores in the sample and their wavelength According to the structure of Esomeprazole magnesium, these will be the expected chromophores. Molecular structure of Esomeprazole magnesium Name chromophore wavelength (nm) Acetylide -C=C 175-180 Aldehyde -CHO 210 Amine -NH2 195 Azo -N=N- 185-400 Carboxyl -COOH 200-210 Ester -COOR 205 Ether -O- 185 Ketone >C=O 195 Nitrate -ONO2 270 Nitrile -C=N 160 Nitrite -ONO 220-230 Nitro -NO2 210 Chromatographic analysis Chromatographic analysis is another technique that would be used to analyze the sample. Chromatography is the ideal method that can help in separating the active and inactive reagents in the process. Different methods can be used in this process. Some of the methods that will be applicable include UV-, Visible- and derivative spectrophotometry and HPLC. The most effective method in this analysis will be HPLC. The analysis will be conducted on a Thermo Separation Products Liquid Chromatography. The sample will be analyzed in the form of esomeprazole magnesium trihydrate. The separations will be conducted at room temperature while using a mobile phase made of acetonitrile/phosphate buffer. The use of this buffer as a mobile phase will provide an elution of active and inactive ingredients from an ODS column with methanol/water (70:30) as the mobile phase (Bol'shakov et al, 2006). Quantitative data from the chromatogram This method will provide an accurate quantitative data because HPLC has been proved to be a simple and stable method for analyzing esomeprazole magnesium trihydrate. The method is precise, accurate and stable and is thus very effective in providing quantitative data in the analysis of the sample (Bard & Faulkner, 2000). Procedure 4 - Data analysis and reporting The data collected using the mentioned will then be gathered in order to record and report the chemical composition of the sample. Both quantitative and qualitative aspects of the compound will reported. In reporting the composition of the sample, the methods will need to be validated for effectiveness and reliability. Validation involves checking certain parameters in collection of data. These parameters include accuracy, precision, robustness and ruggedness. The data collected will be analysed through the use of appropriate statistical tools such as correlation coefficient, regression equation and standard deviation (Holler, et al., 2006). The data will then be recorded in tables, graphs and charts for presentation or reporting. The final report should include both the molecular formula and structure of esomeprazole magnesium for easier understanding. References Bard, A.J.; Faulkner, L.R. (2000). Electrochemical Methods: Fundamentals and Applications. New York: John Wiley & Sons, 2nd Edition, Bol'shakov, Aleksandr A; Ganeev, Aleksandr A; Nemets, Valerii M (2006). "Prospects in analytical atomic spectrometry". Russian Chemical Reviews 75 (4): 289. Ellis LA, Roberts DJ (2007). "Chromatographic and hyphenated methods for elemental speciation analysis in environmental media". Journal of Chromatography A 774 (1–2): 3–19. Holler, F. et al. (2006). Fundamentals of analytical chemistry. Philadelphia: Saunders College Pub Read More