某公司產(chǎn)品質(zhì)量回顧分析報告模版

2012年度產(chǎn)品質(zhì)量回顧分析報告回顧期限：2011年12月－2012年11月編號：ZLHG-BX-2012起草QA簽名：時間：生產(chǎn)部經(jīng)理簽名：時間：研發(fā)部經(jīng)理簽名：時間：審核物控部經(jīng)理簽名：時間：設備部經(jīng)理簽名：時間：質(zhì)量部經(jīng)理簽名：時間：生產(chǎn)負責人簽名：時間：批準質(zhì)量負責人簽名：時間：目錄一、基本情況概述二、生產(chǎn)和質(zhì)量控制情況分析評價1、產(chǎn)品質(zhì)量標準2、產(chǎn)品質(zhì)量回顧3、生產(chǎn)分析4、質(zhì)量事故回顧5、偏差回顧6、超常超標回顧7、穩(wěn)定性試驗8、公用系統(tǒng)、設施設備情況9、變更控制回顧10、委托生產(chǎn)情況回顧11、委托檢驗情況回顧12、不良反應13、產(chǎn)品退貨14、投訴15、產(chǎn)品召回16、藥品注冊相關變更的申報、批準與退審三、結(jié)論一、基本情況概述1概要：根據(jù)2010版GMP要求，結(jié)合《產(chǎn)品年度質(zhì)量回顧分析標準操作規(guī)程》（SOP-ZL-QA-014）的規(guī)定，對 進行產(chǎn)品質(zhì)量回顧分析。本報告抽取在回顧期限所有放行批次的基礎上重點對該品種進行了統(tǒng)計和趨勢分析。2回顧期限：2011年12月1日~2012年11月30日。3生產(chǎn)情況：本回顧年度共放行 藥材細粉118批， 成品105批，總產(chǎn)量為503585（盒），平均收率為95.92%（按放行產(chǎn)量統(tǒng)計）。生產(chǎn)中嚴格按照工藝規(guī)程與標準操作規(guī)程的要求組織生產(chǎn),經(jīng)粉碎、總混、泛丸、干燥、包衣、干燥、選丸、打光、包、外包等工序，完成生產(chǎn)。4規(guī)格與包裝規(guī)格：-包裝：-5有效期與貯藏5.1有效期：24個月。貯藏：密閉，防潮。6產(chǎn)品特點性狀：-功能主治：：-用法用量：-7處方與批量8處方依據(jù)8.1批準文號質(zhì)量標準依據(jù)：---制劑每次投料量： 9生產(chǎn)工藝流程

檢驗檢驗二、生產(chǎn)和質(zhì)量控制情況分析1產(chǎn)品質(zhì)量標準1.1藥材細粉質(zhì)量標準項目名稱控標準法定標準性狀細度細菌數(shù)微生霉菌和酵母菌數(shù)物限大腸菌群度大腸埃希菌活螨1.2成品質(zhì)量標準項目名稱控標準法定標準性狀鑒別檢查水分裝量差異溶散時限細菌數(shù)霉菌和酵母菌數(shù)大腸菌群大腸埃希菌活螨2產(chǎn)品質(zhì)量回顧2.1原輔料購進情況回顧

原輔料供應商入庫批次評價：本回顧年度，供應商質(zhì)量管理均按相關文件嚴格執(zhí)行，供應商質(zhì)量管理的風險處于可控狀態(tài)。2.2原輔料質(zhì)量問題回顧物料名稱供應商不合格批次不合格項目原因處理意見//////評價：本回顧年度購進的原輔料均符合質(zhì)量標準。2.3包裝材料質(zhì)量問題回顧物料名稱供應商不合格批次不合格項目原因處理意見//////評價：本回顧年度購進的包裝材料均符合質(zhì)量標準。2.4中間產(chǎn)品質(zhì)量回顧本回顧年度生產(chǎn)的 藥材細粉所有批次的性狀、細度、微生物限度的檢驗結(jié)果均符合控標準（檢驗結(jié)果詳見QC檢驗報告書），合格率達到100%,可以認為在此工藝條件下生產(chǎn)的產(chǎn)品均能達到產(chǎn)品的質(zhì)量標準。2.5成品質(zhì)量回顧我們對本回顧年度生產(chǎn)的 成品所有批次進行統(tǒng)計和趨勢分析。2.5.1 成品性狀、鑒別、水分、裝量差異、溶散時限、微生物限度、含量檢驗結(jié)果的統(tǒng)計數(shù)據(jù)（檢測結(jié)果來源于該批QC檢驗報告書）。111201符合規(guī)定符合規(guī)定3.8符合規(guī)定26符合規(guī)定8.03.9111202符合規(guī)定符合規(guī)定2.9符合規(guī)定33符合規(guī)定6.34.0111203符合規(guī)定符合規(guī)定4.6符合規(guī)定25符合規(guī)定7.34.4

111204符合規(guī)定符合規(guī)定3.7符合規(guī)定26符合規(guī)定7.64.7111205符合規(guī)定符合規(guī)定3.6符合規(guī)定25符合規(guī)定6.63.8111206符合規(guī)定符合規(guī)定3.5符合規(guī)定26符合規(guī)定7.14.2120101符合規(guī)定符合規(guī)定3.9符合規(guī)定26符合規(guī)定8.04.0120102符合規(guī)定符合規(guī)定3.9符合規(guī)定25符合規(guī)定7.03.9120201符合規(guī)定符合規(guī)定3.5符合規(guī)定32符合規(guī)定6.33.9120202符合規(guī)定符合規(guī)定4.5符合規(guī)定26符合規(guī)定9.44.6120203符合規(guī)定符合規(guī)定5.0符合規(guī)定34符合規(guī)定7.44.3120204符合規(guī)定符合規(guī)定4.3符合規(guī)定35符合規(guī)定7.14.4120205符合規(guī)定符合規(guī)定3.2符合規(guī)定32符合規(guī)定8.05.2120206符合規(guī)定符合規(guī)定3.6符合規(guī)定33符合規(guī)定8.14.2120207符合規(guī)定符合規(guī)定4.1符合規(guī)定26符合規(guī)定7.33.8120301符合規(guī)定符合規(guī)定4.1符合規(guī)定26符合規(guī)定6.64.5120302符合規(guī)定符合規(guī)定4.0符合規(guī)定33符合規(guī)定7.13.9120303符合規(guī)定符合規(guī)定4.7符合規(guī)定35符合規(guī)定5.54.2120304符合規(guī)定符合規(guī)定4.4符合規(guī)定25符合規(guī)定6.44.6120305符合規(guī)定符合規(guī)定3.4符合規(guī)定35符合規(guī)定7.33.8120306符合規(guī)定符合規(guī)定3.1符合規(guī)定25符合規(guī)定5.84.7120307符合規(guī)定符合規(guī)定4.1符合規(guī)定26符合規(guī)定7.14.9120308符合規(guī)定符合規(guī)定4.1符合規(guī)定26符合規(guī)定5.94.2120309符合規(guī)定符合規(guī)定3.2符合規(guī)定26符合規(guī)定6.14.8120310符合規(guī)定符合規(guī)定3.3符合規(guī)定26符合規(guī)定4.44.3120311符合規(guī)定符合規(guī)定3.8符合規(guī)定30符合規(guī)定4.74.4120312符合規(guī)定符合規(guī)定4.5符合規(guī)定26符合規(guī)定4.84.5120601符合規(guī)定符合規(guī)定4.2符合規(guī)定25符合規(guī)定6.64.4120602符合規(guī)定符合規(guī)定3.4符合規(guī)定26符合規(guī)定7.04.6120603符合規(guī)定符合規(guī)定5.1符合規(guī)定30符合規(guī)定7.55.2120604符合規(guī)定符合規(guī)定4.3符合規(guī)定30符合規(guī)定6.54.4120605符合規(guī)定符合規(guī)定4.2符合規(guī)定30符合規(guī)定6.94.6120606符合規(guī)定符合規(guī)定4.1符合規(guī)定30符合規(guī)定8.24.6

120607符合規(guī)定符合規(guī)定4.9符合規(guī)定26符合規(guī)定7.04.6120608符合規(guī)定符合規(guī)定4.1符合規(guī)定26符合規(guī)定6.64.5120701符合規(guī)定符合規(guī)定3.6符合規(guī)定25符合規(guī)定7.23.8120702符合規(guī)定符合規(guī)定3.6符合規(guī)定26符合規(guī)定7.14.2120703符合規(guī)定符合規(guī)定3.8符合規(guī)定30符合規(guī)定7.34.2120704符合規(guī)定符合規(guī)定3.4符合規(guī)定30符合規(guī)定7.24.0120705符合規(guī)定符合規(guī)定4.3符合規(guī)定25符合規(guī)定8.94.8120706符合規(guī)定符合規(guī)定3.5符合規(guī)定30符合規(guī)定9.74.7120707符合規(guī)定符合規(guī)定3.8符合規(guī)定30符合規(guī)定7.95.1120708符合規(guī)定符合規(guī)定4.1符合規(guī)定30符合規(guī)定8.45.1120709符合規(guī)定符合規(guī)定3.9符合規(guī)定30符合規(guī)定7.25.2120710符合規(guī)定符合規(guī)定3.6符合規(guī)定25符合規(guī)定8.95.2120711符合規(guī)定符合規(guī)定4.3符合規(guī)定25符合規(guī)定7.35.7120712符合規(guī)定符合規(guī)定4.8符合規(guī)定26符合規(guī)定6.95.3120801符合規(guī)定符合規(guī)定3.9符合規(guī)定29符合規(guī)定7.45.4120802符合規(guī)定符合規(guī)定4.0符合規(guī)定29符合規(guī)定7.25.4120803符合規(guī)定符合規(guī)定4.8符合規(guī)定30符合規(guī)定9.55.7120804符合規(guī)定符合規(guī)定4.0符合規(guī)定30符合規(guī)定8.85.7120805符合規(guī)定符合規(guī)定4.5符合規(guī)定20符合規(guī)定7.95.0120806符合規(guī)定符合規(guī)定4.8符合規(guī)定26符合規(guī)定8.14.7120807符合規(guī)定符合規(guī)定4.5符合規(guī)定28符合規(guī)定7.85.0120808符合規(guī)定符合規(guī)定4.6符合規(guī)定20符合規(guī)定7.24.9120809符合規(guī)定符合規(guī)定4.2符合規(guī)定25符合規(guī)定8.55.6120810符合規(guī)定符合規(guī)定3.2符合規(guī)定25符合規(guī)定9.14.6120811符合規(guī)定符合規(guī)定3.4符合規(guī)定29符合規(guī)定8.94.4120812符合規(guī)定符合規(guī)定4.0符合規(guī)定25符合規(guī)定8.24.4120813符合規(guī)定符合規(guī)定4.1符合規(guī)定25符合規(guī)定7.74.6120814符合規(guī)定符合規(guī)定4.4符合規(guī)定26符合規(guī)定6.54.6120815符合規(guī)定符合規(guī)定4.4符合規(guī)定25符合規(guī)定7.04.6120816符合規(guī)定符合規(guī)定3.7符合規(guī)定23符合規(guī)定6.74.1

120817符合規(guī)定符合規(guī)定4.4符合規(guī)定26符合規(guī)定7.74.9120818符合規(guī)定符合規(guī)定4.7符合規(guī)定26符合規(guī)定8.35.4120819符合規(guī)定符合規(guī)定3.5符合規(guī)定26符合規(guī)定9.25.6120820符合規(guī)定符合規(guī)定4.2符合規(guī)定25符合規(guī)定8.55.1120821符合規(guī)定符合規(guī)定4.4符合規(guī)定26符合規(guī)定8.95.2120822符合規(guī)定符合規(guī)定4.0符合規(guī)定27符合規(guī)定9.55.7120901符合規(guī)定符合規(guī)定4.8符合規(guī)定25符合規(guī)定8.05.6120902符合規(guī)定符合規(guī)定3.7符合規(guī)定24符合規(guī)定9.05.0120903符合規(guī)定符合規(guī)定5.1符合規(guī)定26符合規(guī)定9.05.5120904符合規(guī)定符合規(guī)定4.1符合規(guī)定36符合規(guī)定9.45.4120905符合規(guī)定符合規(guī)定4.1符合規(guī)定38符合規(guī)定9.84.7120906符合規(guī)定符合規(guī)定3.9符合規(guī)定40符合規(guī)定8.94.9120907符合規(guī)定符合規(guī)定4.8符合規(guī)定25符合規(guī)定9.64.6120908符合規(guī)定符合規(guī)定4.4符合規(guī)定30符合規(guī)定8.64.6120909符合規(guī)定符合規(guī)定3.7符合規(guī)定20符合規(guī)定9.45.0120910符合規(guī)定符合規(guī)定4.6符合規(guī)定28符合規(guī)定8.24.6120911符合規(guī)定符合規(guī)定3.6符合規(guī)定26符合規(guī)定10.14.8120912符合規(guī)定符合規(guī)定3.3符合規(guī)定28符合規(guī)定9.84.9121001符合規(guī)定符合規(guī)定3.2符合規(guī)定20符合規(guī)定9.94.9121002符合規(guī)定符合規(guī)定3.8符合規(guī)定25符合規(guī)定10.95.0121003符合規(guī)定符合規(guī)定4.1符合規(guī)定23符合規(guī)定8.65.0121004符合規(guī)定符合規(guī)定3.3符合規(guī)定30符合規(guī)定10.34.8121005符合規(guī)定符合規(guī)定3.6符合規(guī)定30符合規(guī)定11.45.2121006符合規(guī)定符合規(guī)定4.2符合規(guī)定25符合規(guī)定9.94.7121007符合規(guī)定符合規(guī)定4.2符合規(guī)定25符合規(guī)定8.64.6121008符合規(guī)定符合規(guī)定4.3符合規(guī)定25符合規(guī)定9.44.6121009符合規(guī)定符合規(guī)定4.0符合規(guī)定25符合規(guī)定8.24.8121010符合規(guī)定符合規(guī)定3.8符合規(guī)定28符合規(guī)定8.24.6121011符合規(guī)定符合規(guī)定3.4符合規(guī)定26符合規(guī)定8.74.6121012符合規(guī)定符合規(guī)定3.4符合規(guī)定25符合規(guī)定8.64.6

12n01符合規(guī)定符合規(guī)定4.6符合規(guī)定20符合規(guī)定8.74.412n02符合規(guī)定符合規(guī)定3.7符合規(guī)定28符合規(guī)定7.74.2121103符合規(guī)定符合規(guī)定3.8符合規(guī)定25符合規(guī)定9.14.212n04符合規(guī)定符合規(guī)定3.8符合規(guī)定28符合規(guī)定8.24.6121105符合規(guī)定符合規(guī)定3.6符合規(guī)定25符合規(guī)定8.84.0121106符合規(guī)定符合規(guī)定3.8符合規(guī)定25符合規(guī)定8.64.5121107符合規(guī)定符合規(guī)定3.2符合規(guī)定26符合規(guī)定8.54.5121108符合規(guī)定符合規(guī)定3.3符合規(guī)定30符合規(guī)定9.34.4121109符合規(guī)定符合規(guī)定3.8符合規(guī)定25符合規(guī)定8.44.7121110符合規(guī)定符合規(guī)定3.8符合規(guī)定20符合規(guī)定7.85.0121111符合規(guī)定符合規(guī)定3.8符合規(guī)定26符合規(guī)定7.84.8121112符合規(guī)定符合規(guī)定4.0符合規(guī)定25符合規(guī)定8.64.62.5.2用 成品水分檢驗結(jié)果繪制控制圖。序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)X13.8X234.1X453.6X674.2X894.3X22.9X243.2X464.3X684.4X904.0X34.6X253.3X474.8X694.0X913.8X43.7X263.8X483.9X704.8X923.4X53.6X274.5X494.0X713.7X933.4X63.5X284.2X504.8X725.1X944.6X73.9X293.4X514.0X734.1X953.7X83.9X305.1X524.5X744.1X963.8X93.5X314.3X534.8X753.9X973.8X104.5X324.2X544.5X764.8X983.6X115.0X334.1X554.6X774.4X993.8X124.3X344.9X564.2X783.7X1003.2X133.2X354.1X573.2X794.6X1013.3X143.6X363.6X583.4X803.6X1023.8X154.1X373.6X594.0X813.3X1033.8

X164.1X383.8X604.1X823.2X1043.8X174.0X393.4X614.4X833.8X1054.0X184.7X404.3X624.4X844.1//X194.4X413.5X633.7X853.3//X203.4X423.8X644.4X863.6//X213.1X434.1X654.7X874.2//X224.1X443.9X663.5X884.2//計算平均值為元=3.98；計算移動差距R值如下表:新的子群連續(xù)的對子移動差距R新的子群連續(xù)的對子移動差距R13.82.90.9544.54.60.122.94.61.7554.64.20.434.63.70.9564.23.21.043.73.60.1573.23.40.253.63.50.1583.44.00.663.53.90.4594.04.10.173.93.90.0604.14.40.383.93.50.4614.44.40.093.54.51.0624.43.70.7104.55.00.5633.74.40.7115.04.30.7644.44.70.3124.33.21.1654.73.51.2133.23.60.4663.54.20.7143.64.10.5674.24.40.2154.14.10.0684.44.00.4164.14.00.1694.04.80.8174.04.70.7704.83.71.1184.74.40.3713.75.11.4194.43.41.0725.14.11.0203.43.10.3734.14.10.0

213.14.11.0744.13.90.2224.14.10.0753.94.80.9234.13.20.9764.84.40.4243.23.30.1774.43.70.7253.33.80.5783.74.60.9263.84.50.7794.63.61.0274.54.20.3803.63.30.3284.23.40.8813.33.20.1293.45.11.7823.23.80.6305.14.30.8833.84.10.3314.34.20.1844.13.30.8324.24.10.1853.33.60.3334.14.90.8863.64.20.6344.94.10.8874.24.20.0354.13.60.5884.24.30.1363.63.60.0894.34.00.3373.63.80.2904.03.80.2383.83.40.4913.83.40.4393.44.30.9923.43.40.0404.33.50.8933.44.61.2413.53.80.3944.63.70.9423.84.10.3953.73.80.1434.13.90.2963.83.80.0443.93.60.3973.83.60.2453.64.30.7983.63.80.2464.34.80.5993.83.20.6474.83.90.91003.23.30.1483.94.00.11013.33.80.5494.04.80.81023.83.80.0504.84.00.81033.83.80.0

514.04.50.51043.84.00.2524.54.80.31054.0//534.84.50.3////計算平均移動極差（即這104個值的平均值）=0.498移動極差R控制圖繪制：CLR=R=0.498UCLR=D4R=3.27X0.498=1.63LCLR=D3R=0系數(shù)4和D4的值按9=2行查表得，由于該移動極差圖已呈現(xiàn)出統(tǒng)計控制狀態(tài)，于是可進行單值控制圖的繪圖I 4單值X控制圖繪制： CLx=X=3.98UCLX=X+E2R=X+2.66R=3.98+2.66X0.498=5.31LCLx=X-E2R=X-2.66R=3.98-2.66X0.498=2.66采用n=2,查表知E2=2.66。該控制圖表明過程處于統(tǒng)計控制狀態(tài)。成品水分R控制圖1.81.61.41.21.0D.80.6D.4□.2——CLR0.0——CLR成品水分X控制圖6.0-檢驗結(jié)果6.0-檢驗結(jié)果,匚LXUCLX■ICLXDO0T3Eon二Un口WEETED7IKCIGCIEI《昌二5LWW寸TM口r-JTSCISofT—LEmLss^Tcm二50二I-I昌『IECIED7I—IIEIIL.o.G.Q.0.0,0543210(空)朱黑2.5.3用 成品溶 檢驗結(jié)果繪制控制圖。序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)X126X2426X4726X7025X9325X233X2526X4829X7124X9420X325X2630X4929X7226X9528X426X2726X5030X7336X9625X525X2825X5130X7438X9728X626X2926X5220X7540X9825X726X3030X5326X7625X9925X825X3130X5428X7730X10026X932X3230X5520X7820X10130X1026X3330X5625X7928X10225X1134X3426X5725X8026X10320X1235X3526X5829X8128X10426X1332X3625X5925X8220X10525X1433X3726X6025X8325//X1526X3830X6126X8423//X1626X3930X6225X8530//X1733X4025X6323X8630//

X1835X4130X6426X8725//X1925X4230X6526X8825//X2035X4330X6626X8925//X2125X4430X6725X9025//X2226X4525X6826X9128//X2326X4625X6927X9226//計算平均值為元=27.15;計算移動差距R值如下表:新的子群連續(xù)的對子移動差距新的子群連續(xù)的對子移動差距1263375428208233258552025532526156252504262515725294525261582925462626059252507262516025261825327612625193226662252321026348632326311343516426260123532365262601332331662625114332676725261152626068262711626337692725217333527025241183525107124262192535107226361020352510733638221252617438402

22262607540251523262607625305242626077302010252630478202882630264792826227262518026282282526181282082926304822025530303008325232313030084233073230300853030033302648630255342626087252503526251882525036252618925250372630490252833830300912826239302559226251402530593252054130300942028842303009528253433030096252834430255972825345252509825250462526199252614726293100263044829290101302554929301102252055030300103202665130201010426251

522026610525//5326282////計算平均移動極差（即這104個值的平均值）=3.106移動極差R控制圖繪制：CLr=R=3.106UCLR=D4R=3.27X3.095=10.2LCLr=D3R=0系數(shù)口:和4的值按9=2行查表得，由于該移動極差圖已呈現(xiàn)出統(tǒng)計控制狀態(tài)，于是可進行單值控制圖的繪圖。4單值X控制圖繪制：CLx=X=27.15UCLx-X+E2R=X+2.66R=27.15+2.66X3.106=35.4LCLX=X-E2R=X-2.66R=27.15-2.66X3.106=18.9采用n=2,查表知E2=2.66。該控制圖表明過程處于統(tǒng)計控制狀態(tài)成品溶散時限R控制圖成品溶散時限X控制圖45cclmTcclmT目三□Kim省mETGOEIm.《昌二c-.Lg三寸i二gdkimbo目I■FEET9口glTz三mofl9mLsio二90《MLI—I口ETTT——石蛤站果——石蛤站果一■CLXUCLX一?LCLXo5Q5O5Q5O4332211w后)援fe室使2.5.4用 成品 含量檢驗結(jié)果繪制控制圖。序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)X18.0X246.1X476.9X708.0X938.6X26.3X254.4X487.4X719.0X948.7X37.3X264.7X497.2X729.0X957.7X47.6X274.8X509.5X739.4X969.1X56.6X286.6X518.8X749.8X978.2X67.1X297.0X527.9X758.9X988.8X78.0X307.5X538.1X769.6X998.6X87.0X316.5X547.8X778.6X1008.5X96.3X326.9X557.2X789.4X1019.3X109.4X338.2X568.5X798.2X1028.4X117.4X347.0X579.1X8010.1X1037.8X127.1X356.6X588.9X819.8X1047.8X138.0X367.2X598.2X829.9X1058.6X148.1X377.1X607.7X8310.9//X157.3X387.3X616.5X848.6//X166.6X397.2X627.0X8510.3//

X177.1X408.9X636.7X8611.4//X185.5X419.7X647.7X879.9//X196.4X427.9X658.3X888.6//X207.3X438.4X669.2X899.4//X215.8X447.2X678.5X908.2//X227.1X458.9X688.9X918.2//X235.9X467.3X699.5X928.7//計算平均值為元=7.96；計算移動差距R值如下表:新的子群連續(xù)的對子移動差距R新的子群連續(xù)的對子移動差距R18.06.31.7547.87.20.626.37.31.0557.28.51.337.37.60.3568.59.10.647.66.61.0579.18.90.256.67.10.5588.98.20.767.18.00.9598.27.70.578.07.01.0607.76.51.287.06.30.7616.57.00.596.39.43.1627.06.70.3109.47.42.0636.77.71.0117.47.10.3647.78.30.6127.18.00.9658.39.20.9138.08.10.1669.28.50.7148.17.30.8678.58.90.4157.36.60.7688.99.50.6166.67.10.5699.58.01.5177.15.51.6708.09.01.0185.56.40.9719.09.00.0196.47.30.9729.09.40.4207.35.81.5739.49.80.4

215.87.11.3749.88.90.9227.15.91.2758.99.60.7235.96.10.2769.68.61.0246.14.41.7778.69.40.8254.44.70.3789.48.21.2264.74.80.1798.210.11.9274.86.61.88010.19.80.3286.67.00.4819.89.90.1297.07.50.5829.910.91.0307.56.51.08310.98.62.3316.56.90.4848.610.31.7326.98.21.38510.311.41.1338.27.01.28611.49.91.5347.06.60.4879.98.61.3356.67.20.6888.69.40.8367.27.10.1899.48.21.2377.17.30.2908.28.20.0387.37.20.1918.28.70.5397.28.91.7928.78.60.1408.99.70.8938.68.70.1419.77.91.8948.77.71.0427.98.40.5957.79.11.4438.47.21.2969.18.20.9447.28.91.7978.28.80.6458.97.31.6988.88.60.2467.36.90.4998.68.50.1476.97.40.51008.59.30.8487.47.20.21019.38.40.9497.29.52.31028.47.80.6509.58.80.71037.87.80.0

518.87.90.91047.88.60.8527.98.10.21058.6//538.17.80.3////計算平均移動極差（即這104個值的平均值）=0.8385移動極差R控制圖繪制：CLR=R=0.8385UCLR=D4R=3.27X0.8385=2.74LCLR=D3R=0系數(shù)幺3和D4的值按9=2行查表得，由于該移動極差圖已呈現(xiàn)出統(tǒng)計控制狀態(tài)，于是可進行單值控制圖的繪圖。4單值X控制圖繪制： CLx=X=7.96UCLX=X+E2R=X+2.66R=7.96+2.66X0.8385=10.19LCLx=X-E2R=X-2.66R=7.96-2.66X0.8385=5.73采用n=2,查表知E2=2.66。該控制圖表明過程處于統(tǒng)計控制狀態(tài)。?LCLX成品薯薪里昔元含量X控制圖粘驗必果CLXUCLX0,000002.s8.?LCLX成品薯薪里昔元含量X控制圖粘驗必果CLXUCLX0,000002.s8.6,4,2.MX§3QTmT50031EisaiEOGOEISTMmT30WC寸cimcjetmlEENT口自T?EFTmo(Iss^goETTTmni0,Q.序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)序號數(shù)據(jù)X13.9X234.2X455.2X675.1X894.6X24.0X244.8X465.7X685.2X904.8X34.4X254.3X475.3X695.7X914.6X44.7X264.4X485.4X705.6X924.6X53.8X274.5X495.4X715.0X934.6X64.2X284.2X505.7X725.5X944.4X74.0X294.6X515.7X735.4X954.2X83.9X305.2X525.0X744.7X964.2X93.9X314.4X534.7X754.9X974.6X104.6X324.6X545.0X764.6X984.0X114.3X334.6X554.9X774.6X994.5X124.4X344.6X565.6X785.0X1004.5X135.2X354.5X574.6X794.6X1014.4X144.2X363.8X584.4X804.8X1024.7X153.8X374.2X594.4X814.9X1035.0X164.5X384.2X604.6X824.9X1044.8

X173.9X394.0X614.6X835.0X1054.6X184.2X404.8X624.6X845.0//X194.6X414.7X634.1X854.8//X203.8X425.1X644.9X865.2//X214.7X435.1X655.4X874.7//X224.9X445.2X665.6X884.6//計算平均值為元=4.68；計算移動差距R值如下表:新的子群連續(xù)的對子移動差距R新的子群連續(xù)的對子移動差距R13.94.00.1545.04.90.124.04.40.4554.95.60.734.44.70.3565.64.61.044.73.80.9574.64.40.253.84.20.4584.44.40.064.24.00.2594.44.60.274.03.90.1604.64.60.083.93.90.0614.64.60.093.94.60.7624.64.10.5104.64.30.3634.14.90.8114.34.40.1644.95.40.5124.45.20.8655.45.60.2135.24.21.0665.65.10.5144.23.80.4675.15.20.1153.84.50.7685.25.70.5164.53.90.6695.75.60.1173.94.20.3705.65.00.6184.24.60.4715.05.50.5194.63.80.8725.55.40.1203.84.70.9735.44.70.7214.74.90.2744.74.90.2

224.94.20.7754.94.60.3234.24.80.6764.64.60.0244.84.30.5774.65.00.4254.34.40.1785.04.60.4264.44.50.1794.64.80.2274.54.40.1804.84.90.1284.44.60.2814.94.90.0294.65.20.6824.95.00.1305.24.40.8835.05.00.0314.44.60.2845.04.80.2324.64.60.0854.85.20.4334.64.60.0865.24.70.5344.64.50.1874.74.60.1354.53.80.7884.64.60.0363.84.20.4894.64.80.2374.24.20.0904.84.60.2384.24.00.2914.64.60.0394.04.80.8924.64.60.0404.84.70.1934.64.40.2414.75.10.4944.44.20.2425.15.10.0954.24.20.0435.15.20.1964.24.60.4445.25.20.0974.64.00.6455.25.70.5984.04.50.5465.75.30.4994.54.50.0475.35.40.11004.54.40.1485.45.40.01014.44.70.3495.45.70.31024.75.00.3505.75.70.01035.04.80.2515.75.00.71044.84.60.2

525.04.70.31054.6//534.75.00.3////計算平均移動極差（即這104個值的平均值）=0.3125移動極差R控制圖繪制：CLr=R=0.3125UCLR=D4R=3.27X0.3125=1.02LCLr=D3R=0系數(shù)D3和D4的值按9=2行查表得，由于該移動極差圖已呈現(xiàn)出統(tǒng)計控制狀態(tài)，于是可進行單值控制圖的繪圖14單值X控制圖繪制：CLx=X=4.68UCLx=X+E2R=X+2.66R=4.68+2.66X0.3125=5.51LCLx=X-E2R=X-2.66R=4.68-2.66X0.3125=3.85采用n=2,查表知E2=2.66。該控制圖表明過程處于統(tǒng)計控制狀態(tài)。謗制差距謗制差距R——CLRUCLR■LCLR成品甘草酸含量X控制圖二驗血果,二驗血果,CLXUCIX?LCLXDOCITTETClTClTfTDOCITTETClTClTfT5口口KTZTGOElKClGClfT小昌之m?&fLgox601罟NTbdgclETkclRMTIRCIETD口自TLu9口會官rr-.otroEI息三10二IIQcl.小結(jié)：本回顧年度生產(chǎn)的 所有批次的性狀、鑒別、水分、裝量差異、溶散時限、微生物限度、含量的檢驗結(jié)果來看，均符合控標準，合格率達到100%,可以認為在此工藝條件下生產(chǎn)出的產(chǎn)品均能達到產(chǎn)品的質(zhì)量標準。水分：控標準為不得過7.0%，回顧期限所有數(shù)據(jù)均符合控標準，平均值約為4.0%，合格率達到100%。從控制圖可以看出，各批數(shù)據(jù)基本在控制上線（UCL）與控制下線（LCL）之間，圖型分布也呈正常波動狀態(tài)，認為此工序?qū)λ值目刂铺幵谑芸貭顟B(tài)下，可以認為在此工藝條件下所生產(chǎn)出的產(chǎn)品水分均能達到產(chǎn)品的質(zhì)量標準。溶散時限：控標準為W50min,回顧期限所有數(shù)據(jù)均符合控標準，平均值約為27min,合格率達到100%。從控制圖可以看出，各批數(shù)據(jù)基本在控制上線0CL）與控制下線（LCL）之間，圖型分布也呈正常波動狀態(tài)，認為此工序?qū)θ苌r限的控制處在受控狀態(tài)下，可以認為在此工藝條件下所生產(chǎn)出的產(chǎn)品溶散時限均能達到產(chǎn)品的質(zhì)量標準。薯蕷皂苷元含量：控標準為本品每1g含粉萆薢以薯蕷皂苷元計，不得少于4.2口8。回顧期限所有數(shù)據(jù)均符合控標準，平均值約為8.0mg,合格率達到100%。從控制圖可以看出，各批數(shù)據(jù)偶爾在控制上線（UCL）與控制下線（LCL）之外，可能是藥材產(chǎn)地不固定導致藥材含量不穩(wěn)定，最終導致成品含量的波動。甘草酸含量：控標準為本品每1g含甘草以甘草酸計，不得少于3.71^?；仡櫰谙匏袛?shù)據(jù)均符合控標準，平均值約為4.7mg,合格率達到100%。從控制圖可以看出，各批數(shù)據(jù)偶爾在控制上線（UCL）與控制下線（LCL）之外，可能是藥材產(chǎn)地不固定導致藥材含量不穩(wěn)定，最終導致成品含量的波動。3生產(chǎn)分析3.1關鍵工藝參數(shù)控制情況工序 質(zhì)量控制點質(zhì)量控制項目頻次總混含量、鑒別、混合時間每批泛丸數(shù)量、加水量每批干燥干燥時間、溫度、水分隨時/每批

包衣時間、粘合劑用量、丸重差異隨時包衣丸干燥時間、溫度、水分隨時/每批選丸外觀、丸重差異、鑒別、含量每批包裝外觀、裝量差異、密封性、微生物每批包裝小包裝說明書、數(shù)量、批號隨時/每班中包裝數(shù)量、整齊隨時/每批大包裝數(shù)量、批號、裝箱單（合格證）隨時/每箱3.2產(chǎn)品各工序平衡率平衡率統(tǒng)計表批號總混物料平衡率(%)泛丸、干燥物料平衡率閭選丸物料平衡率(%)包衣、干燥物料平衡率閭擇丸物料平衡率(%)分裝物料平衡率閭包裝物料平衡率閭成品率(%)小盒(%)1111201100.0099.16100.0098.8999.9699.8699.9695.00100.001111202100.0099.5699.9599.0899.9699.3399.9592.70100.001111203100.0099.32100.0099.0099.9699.6499.9693.66100.001111204100.0099.3899.9599.60100.0099.0399.9694.40100.001111205100.0099.43100.0099.46100.0099.5999.9695.50100.00111120699.9599.89100.0099.2899.9799.2199.9695.26100.001120101100.0099.46100.0099.21100.0098.2699.96103.46100.001120102100.0099.40100.0099.28100.0099.4199.96104.54100.001120201100.0099.38100.0098.7299.9698.8099.9586.04100.001120202100.0099.51100.0098.74100.0098.0899.9584.70100.001120203100.0099.57100.0099.14100.0099.8999.9589.00100.001120204100.0098.94100.0098.8999.9699.0499.9584.20100.001120205100.0098.97100.0099.1099.9699.9699.9586.30100.001120206100.0098.75100.0099.1199.9698.9099.9586.80100.001120207100.0099.3299.9598.5299.9698.2399.9583.90100.001120301100.0099.16100.0099.47100.0098.6999.9588.00100.001

120302100.0099.29100.0099.26100.0098.0299.9587.86100.001120303100.0099.40100.0098.9599.9699.2599.9586.64100.001120304100.0099.02100.0099.0799.9698.5299.9585.94100.001120305100.0099.35100.0099.07100.0099.0699.9587.40100.001120306100.0099.51100.0099.16100.0099.6199.9587.32100.001120307100.0099.35100.0098.92100.0099.3699.9587.30100.001120308100.0099.21100.0098.94100.0099.6399.9587.58100.001120309100.0099.27100.0098.89100.0099.5799.9586.98100.001120310100.0099.21100.0099.05100.0099.2499.9585.38100.001120311100.0099.29100.0098.57100.0099.0199.9586.38100.001120312100.0099.35100.0099.18100.0099.0399.9586.44100.001120601100.0099.3599.9799.74100.0099.1999.9592.00100.001120602100.0099.73100.0099.65100.0095.2499.9586.46100.001120603100.0099.67100.0099.36100.0099.3099.9695.52100.001120604100.0098.80100.0099.74100.0099.6299.96101.00100.001120605100.0099.67100.0099.65100.0099.9199.9695.54100.001120606100.0099.46100.0099.80100.0099.1599.9698.14100.001120607100.0099.62100.0099.61100.0098.1699.9590.58100.001120608100.0099.56100.0099.81100.0099.2599.96100.82100.001120701100.0099.40100.0099.74100.0098.8799.96101.00100.001

120702100.0099.57100.0099.81100.0099.9299.96101.00100.001120703100.0099.35100.0099.65100.0099.5199.96101.00100.001120704100.0099.40100.0099.61100.0099.2999.96101.00100.001120705100.0099.57100.0099.55100.0098.3499.96101.00100.001120706100.0099.40100.0099.65100.0099.9799.96103.40100.001120707100.0099.13100.0099.77100.0099.5399.96101.04100.001120708100.0099.40100.0099.81100.0099.2099.96101.04100.001120709100.0099.31100.0099.73100.0099.8599.9698.64100.001120710100.0099.40100.0099.73100.0099.7599.9698.64100.001120711100.0099.49100.0099.21100.0099.8799.9698.64100.001120712100.0099.37100.0099.37100.0099.7399.9698.64100.001120801100.0098.97100.0099.30100.0099.6399.9698.64100.001120802100.0098.74100.0099.27100.0099.8399.9696.24100.001120803100.0099.20100.0099.27100.0099.5199.9696.24100.001120804100.0098.97100.0099.47100.0099.8499.9696.30100.001120805100.0099.08100.0099.60100.0099.5499.9698.70100.001120806100.0099.20100.0099.90100.0099.7499.9698.70100.001120807100.0099.37100.0099.93100.0099.5899.9698.70100.001120808100.0098.97100.0099.80100.0099.6299.9698.60100.001120809100.0098.80100.0099.40100.0099.2799.9698.60100.001

120810100.0098.80100.0099.73100.0099.7399.9698.60100.0011208n100.0098.80100.0099.90100.0099.9699.96101.00100.001120812100.0098.97100.0099.25100.0099.9599.9591.40100.001120813100.0098.86100.0099.28100.0099.8799.9693.80100.001120814100.0098.97100.0099.49100.0099.7999.9591.40100.001120815100.0099.31100.0099.60100.0099.9399.9696.20100.001120816100.0099.09100.0099.27100.0099.8699.9698.60100.001120817100.0098.81100.0099.32100.0098.7399.9693.80100.001120818100.0098.86100.0099.26100.0099.5099.9693.80100.001120819100.0098.76100.0099.26100.0099.5199.9693.80100.001120820100.0098.75100.0099.05100.0099.6899.9591.40100.001120821100.0098.81100.0099.19100.0099.7099.9693.80100.001120822100.0098.70100.0099.32100.0099.8599.9693.80100.001120901100.0098.81100.0099.25100.0099.7299.9693.80100.001120902100.0098.64100.0099.25100.0099.6599.9693.80100.001120903100.0098.87100.0099.32100.0099.8799.9693.80100.001120904100.0098.76100.0099.39100.0099.4199.9693.80100.001120905100.0099.03100.0099.83100.0099.6799.9693.80100.001120906100.0099.25100.0099.59100.0099.9099.7596.00100.001120907100.0098.85100.0099.33100.0099.9499.8996.20100.001

120908100.0098.80100.0099.46100.0099.9499.9696.20100.001120909100.0099.03100.0099.80100.0099.7599.9696.20100.001120910100.0099.37100.0099.63100.0099.3399.9693.80100.001120911100.0099.09100.0099.59100.0099.0399.9693.80100.001120912100.0098.80100.0099.32100.0099.3499.9693.80100.001121001100.0099.09100.0099.32100.0098.9399.9693.80100.001121002100.0098.80100.0099.39100.0098.3299.9591.40100.001121003100.0099.38100.0099.36100.0099.6699.9696.20100.001121004100.0099.06100.0099.41100.0099.7299.9693.80100.001121005100.0099.12100.0099.42100.0099.3999.9696.20100.001121006100.0098.91100.0099.42100.0099.3399.9698.60100.001121007100.0099.12100.0099.62100.0099.2699.9698.60100.001121008100.0099.33100.0099.71100.0099.4199.96101.00100.001121009100.0099.43100.0099.55100.0099.5699.97101.00100.001121010100.0099.17100.0099.52100.0097.3899.9698.60100.001121011100.0099.38100.0099.65100.0099.9999.96101.00100.001121012100.0099.32100.0099.65100.0099.8599.96101.00100.001121101100.0098.96100.0099.47100.0099.2899.96103.40100.001121102100.0099.22100.0099.44100.0099.8699.96105.80100.001121103100.0099.12100.0099.47100.0099.7799.96103.40100.001

12n04100.0099.06100.0099.53100.0099.9899.96105.80100.00112n05100.0099.12100.0099.56100.0095.3699.96101.00100.001121106100.0099.06100.0099.53100.0099.4699.96108.20100.001121107100.0099.06100.0099.53100.0099.8199.96105.80100.001121108100.0099.17100.0099.47100.0099.7999.96108.20100.001121109100.0099.43100.0099.47100.0099.6899.96105.80100.001121110100.0099.01100.0099.44100.0098.2699.96105.80100.001121111100.0099.06100.0099.50100.0099.6599.96108.20100.001121112100.0099.06100.0099.56100.0099.7499.96108.20100.001最大值100.0099.89100.0099.93100.0099.9999.97108.20100.001最小值99.9598.6499.9598.5299.9695.2499.7583.90100.001平均值100.0099.18100.0099.40100.0099.3399.9595.92100.001評價：回顧期限所有放行批次各工序物料平衡率都在合格圍。4質(zhì)量事故回顧:無。5偏差回顧:無。6超常超標回顧OOS編號批號描述涉與批次方案結(jié)果PC-OOS-2012003121204、121205、121206 總混粉的甘草酸含量檢驗結(jié)果出現(xiàn)異常，不符合控標準。3進行實驗室偏差調(diào)查，并安排原樣自復。原樣復檢結(jié)果合格，判定為實驗室偏差。評價：本回顧期限共發(fā)生一起005,已關閉。7長期穩(wěn)定性試驗批號：120201項目（標準規(guī)定）放置時間試驗日期0月3月2012.56月2012.89月2012.11性狀應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定鑒別應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定水分不得過9.0%3.5%4.1%3.6%4.4%裝量差異應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定溶散時限60min32min27min25min27min含量（甘草酸）3.0mg/g3.9mg/g4.1mg/g3.8mg/g4.3mg/g含量（薯蕷皂苷元）4.0mg/g6.4mg/g7.9mg/g6.5mg/g7.9mg/g細菌數(shù)（cfu/g）不得過30000325<1010150霉菌和酵母菌數(shù)（cfu/g）不得過10030<10<10<10大腸菌群（個/g）應〈100<10<10<10<10大腸埃希菌不得檢出未檢出未檢出未檢出未檢出批號：120202放置時間試驗日期項目（標準規(guī)定） 一~^^一0月3月2012.56月2012.89月2012.11性狀 應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定

鑒別應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定水分不得過9.0%4.5%4.5%4.3%4.7%裝量差異應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定溶散時限60min26min27min26min27min含量（甘草酸）3.0mg/g4.6mg/g4.5mg/g4.3mg/g4.4mg/g含量（薯蕷皂苷元）4.0mg/g9.4mg/g7.8mg/g9.3mg/g7.5mg/g細菌數(shù)（cfu/g）不得過300002505535325霉菌和酵母菌數(shù)（cfu/g）不得過100<1015<10<10大腸菌群（個/g）應〈100<10<10<10<10大腸埃希菌不得檢出未檢出未檢出未檢出未檢出批號：120203項目（標準規(guī)定）放置時間試驗日期0月3月2012.56月2012.89月2012.11性狀應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定鑒別應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定水分不得過9.0%5.0%4.5%4.3%4.6%裝量差異應符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定符合規(guī)定溶散時限60min34min28min26min26min含量（甘草酸）3.0mg/g4.3mg/g4.1mg/g4.1mg/g4.2mg/g含量（薯蕷皂苷元）4.0mg/g7.4mg/g7.7m