分析方法验证报告模板

分析方法验证报告模板分析方法验证报告模板 Part ID XXX000066042 41 Chromatogram showedno significantinterference fromsolvent peak 2 Peak ofVitamin Estandard was well resolved from the solventpeak Parameter SpecificationResults PageRepeatibilityRSD 2 0 1 13 2 4Title Validationof dl alpha Tocopherylacetate assayControl Procedure XXX 0000Ingredient Eachcapsule contains800IU ofdl alpha Tocopherylacetate Dateof validation 07 02 xxXXX Pharmaceutical Ltd Analytical MethodValidation ReportPage1of8Validation ReportNo MV 0003 R01Product Vitamin E800IU capsuleBatch No XXXXXNo Acetonitrile Isopropyl alcohol Water 93 7 Lichrospher C18 5um 4 6x250mm 20 L ReproducibilityTheoretical Plate N Tailing Factor T 1 Reproducibility ofResponseMean SD RSD 2 Theoretical Plates The smallestN ofsix injections N 5 54 t a W a h 2 2 16 t a W a 2t aRetention timeof thesolvent WaWidth of the peak atits baseW a h 2Peak widthat halfheight3 Tailing Factor T 1 18 The largestT ofsix injections T W0 05 2f W0 05Width ofpeak a5 heightfDistance between the perpendicular from the peak maximumand the leading edge of thepeak of the1 20of thepeak heightPassFailAdjustment Checked by Performed by16160491615132 1677360 85450 46 6609 00Peak Area16197871601378161385816173221622399Calculation Chromato gram No 01 06 No 1234562N 2 0005798 003T 2 01 13Parameter andResultNo Parameter SpecificationResult1RSD 2 0 0 46 Chromatographic conditionsMobilePhaseColumnFlow Rate1 2mL min DetectorUV 285nm InjectionVolume Standard preparation 205 4mg 50mL x 3mL 25mL 492 96 g mL3 Acetoni trile Fischer Scientific HPLC grade 2 Isopropyl alcoholFischer Scientific HPLC grade 1 d alpha TocopherolSigma W S100 00 57F03031ReagentName ofReagent ManufacturerClass PurityLot No 1Electric balanceJB003 01Satorius BP301S2HPLC JA032 08Shimadzu SPD 10AV VPSystemAnalytical MethodValidation ReportPage2of8Validation ReportNo MV 0003 R01Parameter SystemSuitability Date1 InstrumentNo Name ofInstrument CodeNo Manufacturer TypeXXX Pharmaceutical Ltd 20 L ReproducibilityTheoretical Plate N Tailing Factor T 1 Reproducibility ofResponsePeak AreaMean SD RSD 2 Theoretical Plates The smallestN ofsix injections N 5 54 t a W a h 2 2 16 t a W a 2taRetention timeof thesolvent WaWidth of thepeak atits baseWa h 2Peak widthat halfheight3 Tailing Factor T 1 19 The largestT ofsix injections T W0 05 2f W0 05Widthofpeak a5 heightfDistance betweenthe perpendicularfrom thepeak maximumandtheleading edgeof thepeak of the1 20of thepeak heightPassFailAdjustment Performed byChecked by1633665 66714399 xx 88 6604165214816424731625008163500316 367461610616Calculation ChromatogramNo 26 31 No 1234562N 2 00056093T 2 01 13Parameter andResultNo Parameter SpecificationResult1Specification0 88 Chromatographic conditionsMobilePhase Acetonitrile Isopropyl alcohol Water 93 7 Column Lichrospher C18 5um 4 6x250mm Flow Rate1 2mL min DetectorUV 285nm InjectionVolume Standardpreparation 205 4mg 50mL x 3mL 25mL 492 96 g mL3 Acetonitrile Fischer Scientific HPLC grade 2 Isopropyl alcoholFischer ScientificHPLC grade 1 d alpha TocopherolSigma W S100 00 57F03031No Name ofReagent ManufacturerClass PurityLot No 2HPLC JA032 08Shimadzu SPD 10AV VPSystemReagentNo Name ofInstrument CodeNo Manufacturer Type1Electric balanceJB003 01Satorius BP301S XXX Pharmaceutical Ltd Analytical MethodValidation ReportPage3of8Validation ReportNo MV 0003 R01Parameter SystemSuitability Date2 InstrumentNo Acetonitrile Isopropy l alcohol Water 93 7 LichrospherC18 5um 4 6x250mm 20 L ReproducibilityTheoretical Plate N Tailing Factor T 1 Reproducibility ofResponsePeak AreaMean SD RSD 2 Theoretical Plates The smallestN ofsix injections N 5 54 t a W a h 2 2 16 t a Wa 2taRetention timeof thesolvent WaWidthof thepeak atits baseWa h 2Peak widthat halfheight The largestT ofsix injections T W0 05 2fW0 05Widthofpeak a5 height fDistancebetweentheperpendicularfromthepeakmaximumand theleadingedgeof thepeak of the1 20ofthepeak heightPassFailCheckedby Performedby Adjustment1754883 3319889 2891 13 161573 Tailing Factor T 0 99175739017591441729487174246617520711788742Cal culation Chromatogram No 47 52 No 1234562N 2 00060203T 2 01 08Parameter andResultNo Parameter SpecificationResult1Specification1 13 Chromatographic conditionsMobilePhaseColumnFlow Rate1 2mL min DetectorUV 285nm InjectionVolume5 Standardpreparation 205 4mg 50mL x 3mL 25 mL 492 96 g mL6 4 3 Acetonitrile Fischer ScientificHPLC grade 2 Isopropyl alcoholFischer ScientificHPLC grade 1 d alpha TocopherolSigma W S100 00 57F03031ReagentName ofReagent ManufacturerClass PurityLot No 1Electric balanceJB003 01Satorius BP301S2HPLC JA032 12Shimadzu SPD M10A VPSystemAnalytical MethodValidation ReportPage4of8Validation ReportNo MV 0003 R01Parameter SystemSuitability Date3 InstrumentNo Name ofInstrument CodeNo Manufacturer TypeXXX PharmaceuticalLtd 2 Sartorius Electricbalance Maximum303g d 0 1mg 1 HPLC gradeAcetonitrile2 FischerScientificHPLCgradeMethanol3 Fisc herScientificHPLCgradeIsopropyl alcohol4 FischerScientificHPLCgradewater PassFailCheckedby Performedby4 Forced degradationproductsstressedby Hydrochloricacid Sodium hydroxide fluorescent light heat and hydrogenperoxide donot interferewith thepeakofdl alpha Tocopherylacetate standard Chromatogram No 42 46 Adjustment Chromatogram No 08 09 2 Peak ofdl alpha Tocopherylacetate standardeluated atabout18 6minutes andwaswellresolvedfromthesolvent peak Chromatogram No 11 3 Chromatogram ofVitaminE800IU capsuleis similarto thechromatogramof dl alpha Tocopherylacetate Standard Chromatogram No 10 XXXPharmaceuticalLtd Analytical MethodValidation ReportPage5of8Validation ReportNo MV 0003 R01Parameter Specificity1 Chromatogram showedno significantinterferencefromsolventpeak Linear equation a slope b intercept y ax by X Correlationcoefficientr2 r PassFailAdjustmentCheckedbyPerfo rmedby5 910 4030510081 00001 00003 546 2418269703373 18300 84 728 3224360581 182 085880392 364 161219766Validati on ReportNo MV 0003 R01Parameter LinearityandRange 一 Result r2 0 995 Chromatogram No 12 16 Standard sol Conc g mL Peak areaLinearregressionXXX PharmaceuticalLtd Analytical MethodValidation ReportPage6of8y 3373 4x 18301R 10 0500000 01000000 01500000 02000000 02500000 0300 0000 03500000 00 00200 00400 00600 00800 001000 00Peak AreaConc g mL Linear equation 1 Sample solution Cs x x 50mL xmL 25mL x x 50mL xmL 25mL g mL 2 Sample stock solutionC x x 50mL x x 50mL g mL 3 Result Recovery 100 3 Note 1 C u Au As xCsAu Peak areaofthespiked solutionAs Peak areaofthe Standard solutionCs Concentration oftheStandardsolution 2 Recovery C u C sX100 C u Concentration ofthe Sample solutionPassFailChecked by546 24182 08910 40492 96Adjustment Performedby1615132 167Standard Sample101 96 3 3029106924 52101 55 Average101 181 304115892 8 xx1 96 2 3053664932 02102 37 2 1838277561 07102 71 102 13 3 1815250554 04101 43 99 45 3 585671178 7598 17 1 18299455 58 52102 25 1 596479182 0599 99 2 597735182 44100 20 Conc g mL C u Injection Peak area Cu RecoveryMean Au 4 16173225 16223996 16160491 16197872 16 013783 16138584552 ChromatogramNo 01 06 No 17 25 Conc g mL Cs InjectionPeak areaMean As Spl stocksol factor1000227 60100 00 1000227 6 mg 100 00 10003 0546 24XXX PharmaceuticalLtd Analytical MethodValidation ReportPage7of8Validation ReportNo MV 0003 R01Parameter AuracySpl sol mg factor10003 01 Result RSD 2 0 1 1 1 2 2 2 3 3 3 4 4 4 5 5 5 6 6 6 Mean Mean Mean SD SD SD RSD RSD RSD Mean Me an Mean SD SD SD RSD RSD RSD Mean Mean Mean SD SD SD RSD RS D RSD Mean Mean Mean SD SD SD RSD RSD RSD Mean Mean Mean SD SD SD RSD RSD RSD PassFailInjection 1AdjustmentPerformedby Mean n 9 Intermediateprecision Checked byRepeatibility n 3 Repeatibility n 3 3Repeatibility n 3 20 97 1 04 1 67 0 3631962941 1272548441 8565261520 0035102250 0117742220 0310093710 0011216220 0131738220 0128839470 31 1 16 0 71 1 125491 830991 822241 805620 3614173781 13367669 31 81961763819751103E 0631978273168657Au As0 362630 361200 360421 148871 126663123Peak area636375633868632493xx1391977162Injection123120 001306498 0 0077995070 0190810160 36 0 70 1 02 1 110441 873941 881551 845360 361xx421 1164008871 866951242Au As0 360150 360790 3 62661 125231 1135418242841819xx070036308249730232093123Peak area5900225910795941431843432Injection123120 0037747840 007 2186680 0076029071 03 0 64 0 40 1 123901 882921 890661 8754 50 3669697621 1316869531 8830095741815250304115830536643029 106Au As0 369310 368990 362611 133001 138163123Peakarea5964 7959596458567118299451838277Injection12312Samplesolution Ch romatogram No 17 25 Date Conc g mL 182 08546 24910 407360 85459989 24978719889 28 9070 46 0 61 1 13 1616049161061617887421615132 1671638275 6 17548831617322163500317424661622399163674617520711601378164 24731759144161385816250081729487Standard solutionDateDate1Date2Date3161978716521481757390XXXPharmace uticalLtd Analytical MethodValidation ReportPage8of8Validation ReportNo MV 0003 R01Parameter Precision