產(chǎn)品工藝回顧性驗(yàn)證

1、驗(yàn)證規(guī)程VALIDATION PROCEDURE部門(mén)質(zhì)保部名稱(chēng)產(chǎn)品工藝回顧性驗(yàn)證共2頁(yè)第1頁(yè)編號(hào)PV-02-QA-011/1.0新定修訂號(hào)執(zhí)行日期起草審查批準(zhǔn)批準(zhǔn)日期、驗(yàn)證目的：通過(guò)對(duì)我公司產(chǎn)品回顧性驗(yàn)證，以確認(rèn)目前QA所采取產(chǎn)品生產(chǎn)工藝的可靠性及對(duì)產(chǎn)品質(zhì)量控制點(diǎn)的可行性。、驗(yàn)證內(nèi)容：1、品種與驗(yàn)證項(xiàng)目例：維生素C注射液2ml: 0.5g其它品種工藝回顧性驗(yàn)證同維生素C注射液2、維生素C注射液處方與工藝卡附后；工藝規(guī)程：按SOP操作項(xiàng)目符合標(biāo)準(zhǔn)（可接受標(biāo)準(zhǔn)）含量90.0-110.0%PH5.0-7.0澄明度合格率95%三、驗(yàn)證數(shù)據(jù)分析：對(duì)各項(xiàng)目采用作圖法，確定控制上限和控制下限，驗(yàn)證各數(shù)據(jù)全部

2、在控制上限與控制下限以?xún)?nèi)。若超出范圍，則采取下列措施：1、跟蹤批號(hào)，查找記錄找出偏離原因（原輔料變更：原生產(chǎn)工藝變更）并討論解決。2、生產(chǎn)工藝操作程序，SOP執(zhí)行情況，對(duì)暴露問(wèn)題必須更改。3、內(nèi)控標(biāo)準(zhǔn)不合理必須立即修改，以符合目前工藝實(shí)際要求，保證產(chǎn)品留樣期內(nèi)質(zhì)量穩(wěn) 計(jì)算參考公式:1、移動(dòng)差距：Xn Xn-12、計(jì)算平均值：IX= xi/n3、移動(dòng)極差：MR= n-14、控制 上限：_移動(dòng)差距之和UCL=X+1.88MR 控制下限：LCL=X-1.88MR數(shù)據(jù)圖表：1、表化驗(yàn)日期生產(chǎn)批號(hào)生產(chǎn)數(shù)量含量PH澄明度裝量菌檢2、表二新的子群連續(xù)的對(duì)子移動(dòng)差距123n13、參考圖表nA2D3D421.8

3、8003.26731.02302.57540.72902.28250.57702.11560.48302.00470.4190.0761.92480.3730.1361.86490.3370.1841.816100.3080.2231.777注：我公司對(duì)維生素C注射液驗(yàn)證采用20批。四、驗(yàn)證數(shù)據(jù)及圖表維生素注射液規(guī)格：2ml:0.5g化驗(yàn)日期生產(chǎn)批號(hào)生產(chǎn)數(shù)量(萬(wàn)動(dòng))含量(%)PH澄是度(%)裝量菌檢000805245.3698.016.1496.5合格合格000807245.19597.746.0996.0合格合格000808245.70498.466.0297.0合格合格000809238.

4、97598.106.0097.5合格合格2000.9.9000901245.3397.245.8798.5合格合格000903245.56797.865.8198.5合格合格000904254.18897.425.9198.0合格合格000905254.86297.165.9798.5合格合格00090625535498.106.0098.5合格合格000907254.96598.225.9598.5合格合格2000.10.3000925245.7998.385.9497.0合格合格2000.10.4000926246.20198.825.9698.0合格合格2000.10.400092724

5、5.3499.365.9898.0合格合格2000.10.6000928245.48599.625.9298.0合格合格2000.10.7000929254.41599.365.9197.5合格合格2000.10.8000930254.93499.095.9698.0合格合格001004255.08498.916.0198.0合格合格001005254.91198.736.0697.5合格合格2000.1014001006255.22799.275.9698.0合格合格001103240.58298.476.0997.5合格合格平均98.415.9697.725表二：維生素C注射液含量(2ml

6、:0.5g )新的子群連續(xù)的對(duì)子(%)移動(dòng)差距(%)198.0197.740.27297.7498.460.72398.4698.100.36498.1097.240.86 :597.2497.860.62697.8697.420.44797.4297.160.26897.1698.100.84998.1098.220.121098.2298.380.161198.3898.820.441298.8299.360.541399.3699.620.261499.6299.360.26 :1599.3699.090.271699.0998.910.181798.9198.730.181898.73

7、99.270.541999.2798.470.80移動(dòng)極差：MR =0.27%+0.72%+0.3%+ +0.8%=0 427%19控制限度：平均值文=98.41采用 n=2 查表知 A2=1.88D2=0D4=3.267則：控制上限：UCL=X+1.88MR=99.21%控制下限：LCL=X-1.88MR=97.61%含量偏離控制限度批號(hào)為：批號(hào)含量00901297.24000904297.42000905297.16000927299.36000928299.62表三、維生素929注射液ph(2ml:095g36新 的子群0629連續(xù)的對(duì)子()移動(dòng)差距(%)16.146.090.0526.

8、096.020.0736.026.000.0246.005.870.1355.875.810.0665.815.910.1075.915.970.0685.976.000.0396.005.950.05105.955.940.01115.945.960.0212P5.965.980.02135.985.920.06145.925.910.01155.915.960.05165.966.010.05176.016.060.05186.065.960.10195.966.090.13移動(dòng)偏差:MR=0.05+0.07+0.02+0.13=0.05119控制限度平均值丈=5.96采用 n=2 查表知

9、 A2=1.88D3=0D4=3.267則：控制上限：UCL=X=+1.88MR=6.06控制下限：LCL=X=-1.88MR=5.86PH偏離控制限度批號(hào)為批號(hào)含量00080526.1400080726.0900090325.8100110326.09表四、維生素C注射液PH( 2ml:0.5g)新的子群連續(xù)的對(duì)子(%)移動(dòng)差距(%)196.596.00.5296.097.010.397.097.50.5497.598.51.0598.598.50698.598.00.5798.098.50.5898.598.00.5998.098.50.51098.597.01.51197.098.01.

10、012P98.098.001398.098.001498.097.50.51597.598.00.51698.098.001798.097.50.51897.598.00.51998.097.50.5移動(dòng)偏差：MR=0.5%+1.0%+0.5%+ +0.5%=0.526%19控制限度：平均值攵=97.725%采用 n=2查表知 A2=1.88D3=0D4=3.267則：控制上限：UCL=X+1.88MR=98.71%控制下限：LCL=X-1.88Mr=96.73%澄明度偏離控制限度批號(hào)為：批號(hào)含量000805296.5%五、驗(yàn)證結(jié)果與評(píng)價(jià)維生素C注射液2ml:0.5g，按照QA下發(fā)處方、工藝生產(chǎn)2 0批，其主要質(zhì)量控制項(xiàng) 目含量、PH、澄明度全部符合公司內(nèi)部標(biāo)準(zhǔn)。根據(jù)統(tǒng)計(jì)有下列批號(hào)檢測(cè)項(xiàng)目偏離控制限 度。000901200092720009042含量略低于控制下限0009282含量高于控制上限000905200092920010062原因分析：1、含量略低于控制下限，經(jīng)調(diào)查，含量略低原因?yàn)橥–O2氣體量不足。含量略低,以后生產(chǎn)要調(diào)整通氣量。2、含量高于控制上限，經(jīng)調(diào)查，原因?yàn)榕淞蠒r(shí)用原料反調(diào)PH值，造成含量偏差。00080520008072PH略偏離控制限度00090320011032原因分析：經(jīng)調(diào)查，中間體PH控制靠近內(nèi)控邊沿。0008052000807