The Study On The Related Substance Of Compound Ibuprofen Tablets And Preparation Of The Chemical Composition Of Uncaria

Compound Ibuprofen tablets are compound preparation consisting of ibuprofen andacetaminophen，for pain caused by soft tissue injury, osteoarthritis, rheumatoid arthritis,periarthritis of shoulder. Currently on related substance methods for the determination ofacetaminophen and ibuprofen combination preparations have not been reported in theliterature. To ensure the stability of drug quality control, the subject is detected relatedsubstances in Compound Ibuprofen Tablets by HPLC.Uncaria rhynchophylla(Miq.)Jacks belongs to the Uncaria genus of Rubiaceae family.It distributes mainly in Guangdong， Guangxi， Hunan and Yunnan Provinces. ThePhannacology researeh indieated that the plant of gouteng have the properties of heat-clearing，expelling wind，dilation of blood vessels，regulation of the immune. For decadeswith the continuous progress of extraction and separation methods, chemical compositionstudies on Uncaria has made great achievements.The chemical ingredients isolated fromUncaria including indole alkaloids, triterpenoids, flavonoids, coumarin, quinoline Well acidsaponins, phenols and organic acids. This topic contains the chemical composition ofUncaria system separation to obtain six compounds, and the use of HPLC and TLC puritytesting of each monomer compounds, each compound monomer purity greater than90%.This study was done in the following three steps:A, by selected mobile phase systems of aqueous phosphoric acid-acetonitrile,phosphate-methanol, ammonium acetate-methanol and methanol-water.Finally, determinethe use of phosphate buffer (pH>5.3)aqueous phase and methanol-acetonitrile mixedorganic phase system for determination of compound ibuprofen tablets research relatedsubstances.The best performance liquid chromatography conditions: C18Column(ODS)(4.6 ×150mm，5μm), Column temperature35℃，The detection wavelength225nm；Mobilephase:Mobile phase A is methanol:Acetonitrile(10：90), Mobile phase B is0.05MPhosphate(pH5.8): Mobile phase A(95：5), gradient elution see table3.Second, the establishment of related substances of compound ibuprofen tabletsdetermined by HPLC method durability, such as specificity, accuracy, stability and thelimit of quantification. Durability tests examine chromatography instruments, columns,mobile phase composition, column temperature, flow rate, pH, etc..Compound ibuprofentablets were on acid, alkali, oxidation, temperature, humidity, light and other destructivetests to verify specificity of the method.4-aminophenol,4-chloroacetanilide and4-isobutyl acetophenone was quantified using the external standard method, other singleimpurities and total impurities using quantitative controls the main ingredient.Third, of compound ibuprofen tablets were strong acid, alkali, oxidation, temperature,humidity, light and other destructive testing, and various impurities source attributionanalysis. The results showed that: Compound Ibuprofen tablets in acidic, alkaline andoxidizing conditions, the main component of easily degradable produce new impurities,these new impurities are mainly generated by the acetaminophen, which comes fromacetaminophen impurities of paracetamol can produce damage in acidic and alkalineconditions. At high temperature, light and humidity environment, a more stable compoundibuprofen tablets nature, mainly produced ibuprofen impurities generated underillumination4-isobutyl acetophenone. It should be noted that the storage of drugs prompteddark, dry seal, avoid contact with acids, bases, oxidizing substances.Fourth, Uncaria stem hook5kg, with15times the amount of70%methanol,0.1%HClwas extracted three times, each3h, filtered and the combined extracts three times,recovering the solvent under reduced pressure to obtain a methanol extract of Uncaria. Addwater and mix the extract with concentrated ammonia adjusted to pH9-10, followed bymethylene chloride, n-butanol extraction, solvent recovery, methylene chloride layer, n-butanol layer①, the remaining aqueous HCl tune pH to1, with n-butanol extraction,solvent recovery, n-butanol layer②. The methylene chloride layer and the n-butanol layerwas repeatedly purified by silica gel column chromatography, alumina column chromatography, Sephadex LH-20column chromatography and purified by silica gelchromatography on C18reverse phase separation method to obtain a non-alkaloids andalkaloid.