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Section AP-AV

XXX XX Tablets(60mg)Section AP-AV-FFT

ASSAY/IMPURITIES VALIDATION REPORT

(Section AP-AV-FFBT)FOR

ANALYTICAL METHOD Section AP-R-FFBT

“ANALYTICAL METHOD for XXX XX Tablets(60mg)”

PRODUCT CODE:FFT PRODUCT NAME:XXX XX Tablets,60mg

Batches No.:

20041201,20041202,20041203

1.Method(HPLC)

1.1Chromatographic condition

Column:Diamonsil-C18(5μm,250mm×4.6mm)

Mobile phase:0.05mol/L Sodium Dihydrogen Phosphate[adjust pH to2.5by using Phosphoric acid(1 in10)-methanol(41:59)as mobile phase to perform test.

Detection wavelength:210nm

1.2Linearity

Weigh accurately50mg of XXX XX to a100ml of volumetric flask,dilute to volume with the mobile phase,mix well,accurately transfer a quantity of the solution,prepare a series of concentration of the solutions with mobile phase.Inject10μl of the solutions into HPLC,record the chromatograms and calculate the peak area using external standard method,the results are shown in Table1.

Table1The results of linearity

Section AP-AV

Linearity regression equation:A=71.179C+21.990,r=0.9999.

There is a good linear relationship of the peak area and the concentration within a range of10μg/ml~80μg/ml.

1.3Selectivity/Specificity

Selectivity study has been performed using placebo XXX XX Tablets free of XXX XX.Sample for chromatography has been performed as per method and injected in triplicate.No peaks associated with active ingredient were detected.

In addition,stressed samples of XXX XX Tablets were analyzed using PDA detector,and purity of peak associated with XXX XX has been tested to prove there are no peaks co-eluted with the retention time of Active.

The following stress conditions were applied to samples of XXX XX Tablets:

Take10tablets,powder,weigh five pieces of powder equivalent to4mg of XXX XX to five10ml of test tubes,add the reagents.

a:Acid hydrolysis sample:Add1ml of1.0mol/L Hydrochloric Acid solution,stand for3days,adjust pH to neutral with1.0mol/L Sodium Hydroxide solution,dilute with mobile phase to10ml,mix well,filter. b:Base hydrolysis sample:Add1ml of1.0mol/L Sodium Hydroxide solution,stand for3days,adjust pH to neutral with1.0mol/L Hydrochloric Acid solution,dilute with mobile phase to10ml,mix well, filter.

c:Oxidation hydrolysis sample:Add1ml of30%Hydrogen Peroxide solution,stand for3days,dilute with mobile phase to10ml,mix well,filter.

d:Sun light hydrolysis sample:Being exposed in4500lx±500lx for3days,dilute with mobile phase to 10ml,mix well,filter.

e:Heat hydrolysis sample:Being exposed in105℃for3days,dilute with mobile phase to10ml,mix well,filter.

Resolution between FF peak and most closely eluted impurity peak for each stress condition has been calculated.In addition,purity Factor of FF peak has been determined.

Inject5 l of the solutions into HPLC,the results are shown in Table2.

Table2.The results of stress testing

Section AP-AV

Conclusion:The separation of the peaks of impurities and the major peak of XXX XX meets the related requirement.

1.4Accuracy

Accurately weigh about24mg,30mg,36mg of reference substances to100ml of volumetric flasks,add the excipents according to formulation,dissolve with mobile phase using ultrasonic bath,dilute and volume with mobile phase,mix well,filter.Accurately transfer1ml of the solution to a10ml of volumetric flask,dilute with mobile phase to volume,mix well,as test solution.

In addition,weigh a quantity of reference substance to prepare30μg/ml of solution with mobile phase as standard solution.Inject10μl of solutions above into HPLC,record the chromatograms and calculate the peak area.The results are shown in Table3.

Table3.The results of recovery rate

Section AP-AV

Conclusion:The results demonstrate the recovery rate meet the requirement.

1.5Precision

Weigh accurately a quantity of powder equivalent to30mg of XXX XX under Assay Method,to a100ml of volumetric flask,add the mobile phase using ultrasonic bath,dissolve and dilute to volume with mobile phase,mix well,filter.Transfer1ml of the successive filtrate to a10ml volumetric flask,dilute and volume with mobile phase,as reference solution.

In addition,accurately weigh a quantity of reference substance,dissolve with mobile phase and volume,

prepare a solution of30μg per ml.Then inject10μl of the reference solution and test solution into HPLC respectively,record the chromatograms and calculate the peak area.The results are shown in Table4.

Table4The results of precision

Section AP-AV

Conclusion:RSD is less than1%.The result meets the requirement.

1.6Stability of testing solution

Weigh accurately a quantity of powder equivalent to30mg of XXX XX under Assay Method,to a100ml of volumetric flask,add the mobile phase using ultrasonic bath,dissolve and dilute to volume with mobile phase,mix well,filter.Transfer1ml of the successive filtrate to a10ml volumetric flask,dilute and volume with mobile phase,as reference solution.

In addition,accurately weigh a quantity of reference substance,dissolve with mobile phase and volume, prepare a solution of30μg per ml.Then inject10μl of the reference solution and test solution into HPLC respectively,record the chromatograms and calculate the peak area.At0,624hour,determine the content of XXX XX,the results are shown in Table5.

Table5Stability in solution

Section AP-AV

Conclusion:XXX XX in solution is stable in24hours.

Fig.1XXX XX Reference substance(solvent:ethonal)UV Spectrometry

Fig.2XXX XX Tablets(Bat.No.20030401)(solvent:ethonal)UV Spectrometry

Fig.3XXX XXTablets((Bat.No.20030402)(solvent:ethonal)UV Spectrometry

Fig.4XXX XXTablets((Bat.No.20030403)(solvent:ethonal)UV Spectrometry

Fig.5Excipient(solvent:ethonal)UV Spectrometry

Fig.6XXX XX Reference substance HPLC

Fig.7XXX XX Tablets(Bat.No.20030401)HPLC

Fig.8XXX XX Tablets(Bat.No.20030402)HPLC

Fig.9XXX XX Tablets(Bat.No.20030403)HPLC

Fig.10XXX XX Reference substance(solvent:H2O)UV Spectrometry

Fig.11Excipient(solvent:H2O))UV Spectrometry

Fig.2XXX XX Tablets Blank solvent(H2O)HPLC

Fig.3Excipient(solvent:H2O))HPLC

Fig.14Dissolution profile of XXX XX Tablets

Fig.15Dissolution uniformity profile of XXX XX Tablets(Bat.No.20030401)

Fig.16Dissolution uniformity profile of XXX XX Tablets(Bat.No.20030402)

Fig.17Dissolution uniformity profile of XXX XX Tablets(Bat.No.20030403)

Fig.18Blank solvent(mobile phase)of XXX XX Tablets HPLC

Fig.19XXX XX Tablets Acid hydrolysis HPLC

Fig.20XXX XX Tablets Base hydrolysis HPLC

Fig.21XXX XX Tablets Oxidation hydrosis HPLC

Fig.22XXX XX Tablets Sun light hydrolysis HPLC

Fig.23XXX XX Tablets heat hydrolysis HPLC

Fig.24HPLC of Excipient of XXX XX Tablets

Fig.25XXX XX Tablets related substances self-reference solution(20030401)HPLC

Fig.26XXX XX Tablets related substances self-reference solution(20030402)HPLC Fig.27XXX XX Tablets related

substances self-reference solution(20030403)HPLC

Fig.28XXX XX Tablets(Bat.No.20030401)related substances HPLC Fig.29XXX XXTablets(Bat.No.20030402)related substances HPLC Fig.30XXX XX Tablets(Bat.No.20030403)related substances HPLC