產(chǎn)品工藝回顧性驗(yàn)證規(guī)范

1、驗(yàn) 證 規(guī) 程VALIDATION PROCEDURE部 門(mén)質(zhì)保部名 稱(chēng)產(chǎn)品工藝回憶性驗(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)品回憶性驗(yàn)證，以確認(rèn)目前所采取產(chǎn)品生產(chǎn)工藝 的可靠性及對(duì)產(chǎn)品質(zhì)量操縱點(diǎn)的可行性。驗(yàn)證內(nèi)容：品種與驗(yàn)證項(xiàng)目例：維生素注射液 2ml：0.5g其它品種工藝回憶性驗(yàn)證同維生素注射液。維生素注射液處方與工藝卡附后；工藝規(guī)程：按操作。項(xiàng) 目符合標(biāo)準(zhǔn)（可同意標(biāo)準(zhǔn)）含 量90.0-110.0%5.0-7.0澄明度合格率95%驗(yàn)證數(shù)據(jù)分析：對(duì)各項(xiàng)目采納作圖法，確定操縱上限和操縱下限，驗(yàn)證各數(shù)據(jù)全部在操

2、縱上限與操縱下限以?xún)?nèi)。若超出范圍，則采取下列措施：跟蹤批號(hào)，查找記錄找出偏離緣故（原輔料變更：原生產(chǎn)工藝變更）并討論解決。生產(chǎn)工藝操作程序，執(zhí)行情況，對(duì)暴露問(wèn)題必須更改。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)定。計(jì)算參考公式：移動(dòng)差距：XnXn-1移動(dòng)差距之和計(jì)算平均值：Xxi/nn-1、移動(dòng)極差：MR= 、操縱上限：UCL=X+1.88MR操縱下限：LCL=X-1.88MR數(shù)據(jù)圖表：表一化驗(yàn)日期生產(chǎn)批號(hào)生產(chǎn)數(shù)量含量澄明度裝量菌檢、表二新的子群連續(xù)的對(duì)子移動(dòng)差距n、參考圖表nA2D3D421.88003.26731.02302.57540.72902.282

3、50.57702.11560.48302.00470.4190.0761.92480.3730.1361.86490.3370.1841.816100.3080.2231.777注：我公司對(duì)維生素注射液驗(yàn)證采納批。四、驗(yàn)證數(shù)據(jù)及圖表 維生素注射液規(guī)格：2ml:0.5g表一：化驗(yàn)日期生產(chǎn)批號(hào)生產(chǎn)數(shù)量（萬(wàn)動(dòng)）含量（）澄是度（）裝量菌檢2000.83698.016.1496.5合格合格2000.819597.746.0996.0合格合格2000.8.16000808245.70498.466.0297.0合格合格2000.8/p>

4、.97598.106.0097.5合格合格2000.9.9000901245.3397.245.8798.5合格合格2000.9.11000903245.56797.865.8198.5合格合格2000.9.12000904254.18897.425.9198.0合格合格2000.986297.165.9798.5合格合格2000.9.1400090625535498.106.0098.5合格合格2000.996598.225.9598.5合格合格2000.10.3000925245.7998.385.9497.0合格合格2000.10.40

5、00926246.20198.825.9698.0合格合格2000.10.4000927245.3499.365.9898.0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2000.10.12001004255.08498.916.0198.0合格合格2000.1091198.736.0697.5合格合格2000.1014001006255.22799.275.9698.0合

6、格合格2000.1158298.476.0997.5合格合格平均98.415.9697.725表二：維生素注射液含量（2ml:0.5g）新的子群連續(xù)的對(duì)子(%)移動(dòng)差距(%)98.0197.740.2797.7498.460.7298.4698.100.3698.1097.240.8697.2497.860.6297.8697.420.4497.4297.160.2697.1698.100.8498.1098.220.1298.2298.380.1698.3898.820.4498.8299.360.5499.3699.620.2699.6299.360.2699.3

7、699.090.2799.0998.910.1898.9198.730.1898.7399.270.5499.2798.470.80移動(dòng)極差：MR =0.27%+0.72%+0.3%+0.8%=0.427%= 19操縱限度：平均值98.41=采納n=2 查表知A2=1.88 D2=0 D4=3.267=則：操縱上限：UCL=X+1.88 MR=99.21%操縱下限：LCL=X-1.88 MR=97.61%含量偏離操縱限度批號(hào)為： 批號(hào) 含量 009012 97.24 0009042 97.42 0009052 97.16 0009272 99.360009292 99.360010062 99

8、.27 0009282 99.62 表三、維生素注射液（2ml:0.5g）新的子群連續(xù)的對(duì)子(%)移動(dòng)差距(%)6.146.090.056.096.020.076.026.000.026.005.870.135.875.810.065.815.910.105.915.970.065.976.000.036.005.950.055.955.940.015.945.960.025.965.980.025.985.920.065.925.910.015.915.960.055.966.010.056.016.060.056.065.960.105.966.090.13移動(dòng)偏差：MR=0.05+0.0

9、7+0.02+0.13=0.051 19=操縱限度：平均值5.96=采納n=2 查表知A2=1.88 D3=0 D4=3.267=則：操縱上限：UCL=X+1.88MR=6.06 操縱下限：LCL=X-1.88MR=5.86PH偏離操縱限度批號(hào)為 批號(hào) 含量 0008052 6.14 0008072 6.09 0009032 5.81 0011032 6.09表四、維生素注射液（2ml:0.5g）新的子群連續(xù)的對(duì)子(%)移動(dòng)差距(%)96.596.00.596.097.010.97.097.50.597.598.51.098.598.5098.598.00.598.098.50.598.598

10、.00.598.098.50.598.597.01.597.098.01.098.098.0098.098.0098.097.50.597.598.00.598.098.0098.097.50.597.598.00.598.097.50.5移動(dòng)偏差：MR=0.5%+1.0%+0.5%+0.5%=0.526% 19=操縱限度：平均值97.725%采納n=2 查表知A2=1.88 D3=0 D4=3.267則：操縱上限：UCL=X+1.88MR=98.71%操縱下限：LCL=X-1.88MR=96.73%澄明度偏離操縱限度批號(hào)為： 批號(hào) 含量 0008052 96.5% 0008072 96.0%五、驗(yàn)證結(jié)果與評(píng)價(jià)維生素注射液2ml:0.5g，按照下發(fā)處方、工藝生產(chǎn)批，其要緊質(zhì)量操縱項(xiàng)目含量、澄明度全部符合公司內(nèi)部標(biāo)準(zhǔn)。依照統(tǒng)計(jì)有下列批號(hào)檢測(cè)項(xiàng)目偏離操縱限度。0009012 00092720009042 含量略低于操縱下限 0009282 含量高于操縱上限0009052 0009292 0010062緣故分析：、含量略低于操縱下限，經(jīng)調(diào)查，含量略低緣故為通氣體量不足。含量略低，以后生產(chǎn)要調(diào)整通氣量。 、含量高于操縱上限，經(jīng)調(diào)查，緣故為配料時(shí)用原料反調(diào)值，造成含量偏差。00080520008072 略偏離操縱限度00090320011032緣故分析：經(jīng)調(diào)查，中間體操縱靠近內(nèi)控邊