Confirm The Chemistry Structure Of Amlexamox And Study Quality Standards

Objective1.Confirm the chemistry structure of Amlexamox.2. Study quality of Amlexamox, establish quality control standards.3. Study stability of Amlexamox, determine it's validity period. Methods1. Chemistry structure study: under the same condition, testing the sample and control sample with infrared absorption spectrum; ultraviolet visible spectrophotometer, nuclear magnetic resonance; mass spectrometric. Element analysis; X-ray diffraction; quantitative differential thermal analysis were used to test the sample.2. Quality study: according to the china pharmacopoeia appendix,testing the melting point; solubility; ultraviolet absorptivity. With High performance liquid chromatography; gas chromatography were used to check the impurity. Draw up analytical method and limitation of related substance and decompose product. Non-aqueous titration was used to test the content with methanol sodium3. Stability study: carrying out affect factor and acceleration experiment witheffulgence, high temperature and high humidity. High performance liquid chromatography was used to test the appearance, content, decompose product, which remaining at room temperature for 3 years. Results and Conclusions1. Molecule structure1. 1 Element analysis proved that the sample contains the element of C, H, N, 0, the ratio is accordance with C16H14N204.1.2. Mass spectrometric analysis proves that the m/z of ion peak is 298, which is accordance with C16II14N204.1.3 The molecule of Amloxamox is even number, it demonstrate the number of atom N is even. 2. Main group and the molecule structure2. 1 According to the ratio of C and H, the sample may be aromatics compound, it also can be proved by that: (a) saturation(Ω)Ω = (2+2N4+N3-N10 ) / 2 = (2+2X16+2-14) / 2 = 11The saturation of Amlexamox is 11, a benzene ring has four unsaturated units, two benzopyridine rings have six unsaturated units, a carbonyl has one. It is supposed that it has 3 benzopyranopyridine and one carboxyl.(b)Ultraviolet spectrum showed the K absorption of ether, B absorption of benzene ring, R absorption of pyridine.(c)IR spectrum show that 1606,1581,1482 cm-1 are the feature absorption of benzene ring ,820cm is 1,2,4—trisubstitute benzene .(d)0n 1HNMR spectrum, δ 7. 5-8. 7 are four group poly-peak, these are H of benzene ring and pyridine rings. 0nl3CNMR,spectrum δ 105. 8-161. 3 also prove the existence of benzene ring .3. IR spectrum show that 1675, 1670cm-lare stretching vibration of C=0, so carboxyl and carbonyl are exist, 13CNMR spectrum show δ 167. 8, 174. 68 are carbon of carboxyl and carbonyl, the peak width of 1HNMR δ 13.5 is H of carboxyl.4. Losing methyl come into being the base peak of m/z 283, and get bigger ion fragment. On 1HNMR spectrum the double peak of 8 1. 2 is two H proton of two methyl, on 13CNMR spectrum , δ 23. 64 is C of saturation methyl. These proves methyl exist in the structure.5.On IR spectrum, 3317, 3207cm-lare extend vibration of N-H boned in amino, 1272cm-lis C-N extend vibration of C-N boned. On 1HNMR spectrum the width of δ 8. 2 are two H proton of amino.6. On IR spectrum, 1237cm-1 is extend vibration of -0-.So Amlexamox is a aromatics compound, it contains benzopyrano[2, 3, -bjpyridine, carboxyl and carbonyl, methyl and carbonyl, methyl and amino each group connect with benzene ring respectively. MS: the bigger ion fragment of m/z283, 240, 222 can show that the molecule structure is 7. Solubility, Amlexamox is dissolved in DMF, hardly dissolved in methanol and water, the sulfate must less 0. 15%, losing on drying is less than 0. 1%, residue on ignition is less than 0. 10%, heavy metal is less than 10ppm, DMF is less than 0.088%(g/g), the limitation of assay is no less than 98.5%. These standards can control the quality of Amlexamox precise .8. Affect trial showing that, the index has less transformation under effulgence, high temperature and high humidity. It is stable . Remaining the sample at 40 °C,RH75% condition, the index has less transformation. The analysis index has less transformation by remaining sample at room temperature. So the availability of Amlexamox is three years.