| According to existent question on analytical method of metamizole sodium related substance in the actual mass control. First carry on a composition preparation about internal standard substance and carry on chemistry structure to belong.Then as to it's the analytical method carry on an excellent condition for turning a select, finding out the best measuring, and vs draft of analytical method progress methodology verification. Finally an question vs metamizole sodium raw material medicine have unknown impurity progress chemistry structure validation, and random sample metamizole sodium to carry on a measuring, with what investigation analyze method at physically applied amid of feasibility.First aim at metamizole sodium medium body carry on a composition preparation, and adopt MS, IR, UV aim to carry on the structure confirm. Secondly to create metamizole sodium the best analysis method concerning matter mass control, to carry on strong acid, strong alkali, thermal, shine, oxadation etc. destructive test on the metamizole sodium, aim at each condition down generate of impurity, vs measuring condition progress excellent turn a select, include vs chromatographic column, run phase, wavelength etc., initial establish the HPLC chromatographic condition. At the same time vs recognize of analyze method progress specialization, accuracy, precision,linearity and range, durability, limit of detection,_limit of quantitation. Finally vs unknow impurity of metamizole sodium raw material medicine progress structure validation, pass adopting the chromatographic data investigation and LC-MS allied use a technique, provide an accurate information for the structure that unknown impurity. Random sample metamizole sodium raw material medicine completed product, according to create of analytical method progress measuring, investigate the contents of each impurity in the metamizole sodiumr raw material medicine.Pass the composition preparation and structure validation that the metamizole sodium medium body, can provide standard substance for next move of analytical investigation.Pass destructiveness test, discover that metamizole sodium in the sunlight irradiation,_ultraviolet irradiation, heat, acid, alkali, oxidize matter condition down the instability, can generate more catabolite.Aim at all impurities progress selection about chromatographic condition, get the best HPLC condition as follows:Wavelength 254 nm; Chromatographic column:ODS C18 (4.6x250mm,5μm);Mobile phases:a mixture of 30 volumes of methanol and 70 volumes of a buffer solution prepared by adjusting a mixture of 1000 volumes of a 6.0g/l solution of sodium dihydrogen phosphate and 1volumes of triethylamine to pH 7.0 with strong sodium hydroxide solution.Pass the Validation of Analytical Methods, verification that specialization, accuracy, precision,linearity and range, durability of method_meet the specification, and high sensitivitys,at the same time prove the metamizole sodium very soluble in water and born impurity,prepare the solution immediately before use.Then aim at unknow impurity of metamizole sodium raw material medicine, adopt two kinds of paths progress structure validation,one pass adopting the chromatographic data investigation, know that retention time of unknown impurity in accord with retention time of metamizole sodium medium body, two adopt LC-MS allied use a technique, receive two unknown impurity mass chromatogram and comprehensive analysis,further recognized to the molecular weight and structure type of unknown impurity, explained that unknown impurity of metamizole sodium root in material medicine medium body. Finally from the test result of metamizole sodium sample enunciation, this method applicable to quality controll of the metamizole sodium completed product.The method can be been used to determine metamizole sodium related substances, and accurate measure the content of all impurities, the analytical method is rapid, simple, accuracy, and can be used for the quality controll of the metamizole sodium completed product. |
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