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Acetonitrile Lab Report

1692 Words7 Pages

2.2 Chemicals and reagents The API of AN (99.9% pure) 1000mg was purchased from market. HPLC grade acetonitrile (SD fine limited). Analytical grade hydrochloric acid ,sodium hydroxide flakes, hydrogen peroxide. Milli-Q Water purchased from market.. 2.3 Details of Method Chromatographic conditions: Reversed Phase High Performance liquid chromatography method with UV detection separation was achieved on zorbox Agilent Eclipsc XDB column c18(150 nm× 4.6 mm×5µm) as stationary phase with binary gradient mode solvent phase A. Composed of H3PO4(ortho phosphoric acid ) buffer ( pH ≈2, 0.02M) and phase B as Acetonitrile ,The Flow rate of the mobile phase was 1.0 mL/min and the total elution time including the column re-equilibration was approximately …show more content…

This clearly indicated addition of H2O molecule to the drug. As the Application of nitrogen rule and proposed the presence of even nitrogen ie, C12H15NO4 (Theoretical mass 237.10) as the most probable molecular formula. Degradation product 02 is generated from the drug by simple amide hydrolysis in basic condition. Since Degradation product 02 was formed in basic, It was observed that, AN undergoes base hydrolysis. Degradation study of Product 01 using Aqueous 1N NaOH solution .The mechanism is operated by hydrolysis. The hydroxyl group (-OH) of NaOH attacks an electrophilic carbon of >C=O group which an removal of tertiary Nitrogen gives 4-MBA and PD as by products. Degradation study of Product 02 using Aqueous 1N NaOH solution . The mechanism is operated by hydrolysis. The hydroxyl group (-OH) of NaOH attacks an electrophilic carbon of >N-C=O which as rearrangement gives carbonial . This carbonial abstract proton from water to give NAG. The established over degradation of NAG to 4-MBA was also obseved in alkali condition. Degradation pathway of AN is shown in Fig.3. The isolated degradation products are subjected to Mass studies to obtain their accurate mass fragment patterns. Which help to design tentative structure of degradation products which are confirmed by 1H NMR and IR. On the basis of results complete degradation path for AN has been established. We have also

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