對照品管理SOP雙語

1、起草/修訂人：Author日期：Date部門主管審查：Dept. Head Approval日期：DateQA批準(zhǔn)：Approved by QA日期：Date分 發(fā)：Distribution:QA, QC, R&D目的：描述化驗(yàn)室對照品的接收、確認(rèn)、貯存、庫存、分發(fā)、使用的規(guī)程。PURPOSE:This procedure describes a process used by Lab operation for the receipt, qualification, storage, inventory, distribution and use of analytical refe

2、rence standard范圍：適用于化驗(yàn)室內(nèi)所用的對照品，包括基準(zhǔn)對照品、第二對照品。SCOPE:This procedure is applicable to analytical reference standards used in QC lab, includes the Primary Reference Standards and the Secondary Reference Standards參考文件：REFERENCE AND ATTACHMENT:SOP/題目 SOP/TITLE記錄/附件/題目 FORMS/ATTACHMENTS/TITLE3-0002OOS調(diào)查附件1

3、：對照品標(biāo)簽樣例Investigation of Out-of-Specification ResultAttachment 1: Reference Standard Label (Example)F-03-010對照品登記臺帳Reference Standard Inventory Log SheetF-03-011對照品接收記錄Reference Standard Receiving LogbookF-03-012對照品使用記錄Use Record of Reference Standard 定 義：DEFINITIONS:基準(zhǔn)對照品以廣泛分析表明具有可信的、高純度的物質(zhì)。這類標(biāo)準(zhǔn)品可以

4、：1）來源于法定機(jī)構(gòu)；2）獨(dú)立合成；3）來自于高純度的現(xiàn)有生產(chǎn)物料；4）用進(jìn)一步精制現(xiàn)有生產(chǎn)物料的方法來制備。Reference Standard, Primary A substance that has been shown by an extensive set of analytical tests to be authentic material that should be of high purity. This standard could be: (1) obtained from an officially recognized source, (2) prepared b

5、y independent synthesis, (3) obtained from existing production material of high purity, or (4) prepared by further purification of existing production material.第二對照品與基準(zhǔn)對照品比較顯示有規(guī)定的質(zhì)量和純度，并用作日常檢驗(yàn)分析的參考標(biāo)準(zhǔn)品。Reference Standard, Secondary A substance of established quality and purity, as shown by comparison

6、 to a primary reference standard, used as a reference standard for routine laboratory analysis.規(guī) 程：PROCEDURE:責(zé) 任 人操 作RESPONSIBILITYACTION1.對照品接收RECEIPT OF REFERENCE STANDARDQC主管1.1QC主管指定專人負(fù)責(zé)對照品的管理；對照品管理員負(fù)責(zé)對照品的接收、貯存以及發(fā)放等的管理。QC SupervisorQC Supervisor designee is responsible for the management of all

7、reference standards, such as the receipt, storage and distribution of reference standard.對照品管理員1.2接收對照品時，應(yīng)檢查對照品的包裝是否完好、是否提供檢驗(yàn)報(bào)告書、檢驗(yàn)報(bào)告書是否與實(shí)物相符，等等。Control ClerkUpon receipt, verify the package of the reference standards, confirm whether the certificate of analysis is available, and the reference stand

8、ards received are the same as the certificate of analysis, etc.1.3將對照品的相關(guān)信息在對照品登記臺帳上作好記錄，每批對照品建立一份管理臺帳。Enter reference standard information into the Reference Standard Receiving logbook, and establish a Reference Standard Inventory log sheet for each lot. 1.4接收后的對照品給定公司內(nèi)批號。Assign the lot number for

9、received reference standards對照品的批號由：類別號年號流水號組成：The lot number is consist of: Sort number + digit number of the calendar Year + sequential number:.1類別號：Sort number.1.1基準(zhǔn)對照品：RSP（Reference Standard, Primary）.1.2第二對照品：RSS（Reference Standard, Secondary）.2年號：用2位數(shù)的年份表示Year: 2 digit number of the year desig

10、nation.3流水號：用2位數(shù)字表示。Sequential number: 2 digit number.1.5對照品接收后，在每批對照品的每個包裝上貼簽（附件1），標(biāo)明名稱、批號、數(shù)量、來源、瓶號/總瓶數(shù)（比如，共有10瓶，其中第2瓶為：2/10）、接收人簽名/日期等內(nèi)容。At time of receipt, label each standard container (attachment 1), with the reference standard name, lot number, quantity, source, container number/total containe

11、rs number (e.g., the total container is 10 bottles, then second bottle is 2/10), and initial and date of the receiver.責(zé) 任 人操 作RESPONSIBILITYACTION對照品管理員1.6將對照品放入標(biāo)有“待確認(rèn)對照品”的干燥器中，存放于28冰箱中，或者存放于對照品所規(guī)定的貯存條件。Control ClerkPlace reference standard into desiccator (marked with “Reference Standard, to be qua

12、lified”) in refrigerator (temperature controlled within 2 to 8 Degree C), or place in required storage condition in accordance with reference standard.1.7對照品應(yīng)存放于棕色玻璃瓶中，對于不符合此要求的，在接收后，將對照品裝入或分裝于棕色玻璃瓶中。The reference standard should be stored in brown glass bottles. If it is found not meeting the requi

13、rement, it should be placed into or subdivided into brown glass bottles after receipt.2.對照品確認(rèn)QUALIFICAITON OF REFERENCE STANDARDSQC2.1對照品應(yīng)從法定機(jī)構(gòu)購買（如，USP、EP、CP等）；并且，只要是適用的，內(nèi)部使用的對照品應(yīng)根據(jù)這些從法定機(jī)構(gòu)購買來的對照品進(jìn)行確認(rèn)。如果法定對照品不能得到，則內(nèi)部使用的對照品必須根據(jù)一個確認(rèn)的標(biāo)準(zhǔn)品進(jìn)行確認(rèn)，或必須根據(jù)本SOP中下面的要求的進(jìn)行全部的確認(rèn)。Reference standards should be purchase

14、d from an officially recognized source (e.g., USP, EP, and CP) and in-house reference standards should be qualified against them, whenever applicable. If officially reference standard is not available or applicable, in-house reference standards must be qualified against a qualified standard or full

15、qualification must be performed according to the following requirement of this SOP.2.2對照品的確認(rèn)包括：The qualification of reference standard includes:2.2.1基準(zhǔn)對照品的確認(rèn)Qualification of Primary Reference Standard2.2.2第二對照品的確認(rèn)Qualification of Secondary Reference Standards2.2.2.1根據(jù)法定對照品（如，USP、EP、CP等）或其他已確認(rèn)的標(biāo)準(zhǔn)，對內(nèi)部

16、使用的對照品的確認(rèn)。Qualification of in-house reference standards against an official reference standard (e.g., USP, EP, CP, etc.) or other qualified standard.2.2.2.2當(dāng)沒有法定對照品（如，USP、EP、CP等），或其他已確認(rèn)的對照品時，內(nèi)部使用的對照品的確認(rèn)。Qualification of an in-house reference standard when official reference standard (e.g., USP, EP,

17、CP, etc.), or other qualified standard is not available.責(zé) 任 人操 作RESPONSIBILITYACTIONQC, QA2.3基準(zhǔn)對照品的確認(rèn)Qualification of Primary Reference Standard2.3.1從法定機(jī)構(gòu)購買的基準(zhǔn)對照品，在根據(jù)“1. 接收”的規(guī)程接收后，將與該批對照品有關(guān)的資料轉(zhuǎn)至QA審核。經(jīng)QA審核后，發(fā)放檢驗(yàn)報(bào)告書。The primary reference standard purchased from officially recognized source. After refe

18、rence standard has been received according to the requirement of “1. Receipt of Reference Standard”, submit the documents related to that batch reference standard to QA for review. After review, QA shall issue the certificate of analysis.2.4根據(jù)法定對照品（如，USP、EP、CP等）或其他已確認(rèn)的標(biāo)準(zhǔn)，對內(nèi)部使用的對照品的確認(rèn)Qualification of

19、 in-house reference standard against an official reference standard (e.g., USP, EP, CP, etc.) or other qualified standard:2.4.1起草一份對照品的確認(rèn)方案，方案包括下面的信息：Prepare a qualification protocol of reference standard, including the following information:2.4.1.1物料的鑒別，包括來源（如，生產(chǎn)廠家）以及批號。Identification of the materi

20、al, including source (e.g., manufacturer) and lot number.2.4.1.2檢驗(yàn)報(bào)告書：檢驗(yàn)報(bào)告書應(yīng)包括所有法定對照品的檢驗(yàn)結(jié)果，若適用。如果沒有，或如果生產(chǎn)廠家的檢驗(yàn)報(bào)告書事先沒有驗(yàn)證，則完整的法定對照品的檢驗(yàn)是必需的，檢驗(yàn)可以在公司內(nèi)完成，也可以由批準(zhǔn)的公司外的適當(dāng)?shù)膶?shí)驗(yàn)室完成。物料必須符合所有的檢驗(yàn)要求。如果沒有法定對照品，則該建議的內(nèi)部使用的對照品必須符合所有適用的質(zhì)量標(biāo)準(zhǔn)。Certificate of Analysis: the COA should include results from all official RS test

21、s, when applicable. If it dose not or if the manufacturers COA has not been previously validated, then complete official RS testing is necessary and may be performed in-house or by an approved and appropriate outside laboratory. The material must pass all test requirements. When official RS is not a

22、pplicable, the proposed in-house reference standard must meet all applicable specifications.2.4.1.3用于對比的法定對照品或其他已確認(rèn)的對照品的鑒別。Identity of official reference standards or other qualified reference standard used for comparison.責(zé) 任 人操 作RESPONSIBILITYACTION2.4.1.4檢驗(yàn)方法和結(jié)果：內(nèi)部使用的對照品的檢驗(yàn)通常應(yīng)包括其所使用時的方法。在確認(rèn)之前，建議的內(nèi)

23、部使用的對照品應(yīng)采用法定對照品或其他已確認(rèn)的對照品一致的方法進(jìn)行干燥，若適用。Methods of Analysis and Results: testing in-house reference standard should always include the method for which it is to be used. The proposed in-house reference standard, when applicable, should be dried in the same manner as the official RS or other qualified

24、 RS prior to qualification.2.4.1.4.1根據(jù)內(nèi)部使用的對照品所要用于檢驗(yàn)的，所適用的產(chǎn)品的方法中標(biāo)準(zhǔn)溶液的配制方法，對內(nèi)部使用的對照品，以及法定或其他已確認(rèn)的對照品進(jìn)行檢驗(yàn)。Test proposed in-house reference standard according to the method for which it shall be used by following only the standard preparation procedure in the applicable product for both the proposed in-

25、house reference standard and the official or other qualified reference standard.2.4.1.4.2線性：根據(jù)建議的對照品所要用于的方法，配制三個溶液。根據(jù)方法中所規(guī)定的范圍限度，配制高、中、低三個濃度的溶液。如果范圍沒有規(guī)定，則在目前水平的±15%配制。用同樣的方法配制法定對照品或其他已確認(rèn)的對照品。檢測儀器對所有溶液的三個讀數(shù)的響應(yīng)，按面積歸一化法計(jì)算。相關(guān)系數(shù)（r2）應(yīng)³ 0.995。Linearity: Prepare three concentrations of the propose

26、d standard material according to the method for which it is to be used. Prepare these solutions at the upper, mid and lower limit of the range specified in the method. If a range is not specified, prepare solutions at ±15% of the target level. Prepare the official RS or other qualified RS in th

27、e same manner. Measure instrument response for three readings of all solutions and perform least squares fit analysis. The correlation coefficient (r2) should be ³ 0.995.責(zé) 任 人操 作RESPONSIBILITYACTION2.4.1.4.3含量：根據(jù)所要用于的方法，配制五份待確認(rèn)對照品的溶液（雙人）。用同樣的方法配制法定對照品或其他已確認(rèn)的對照品溶液。結(jié)果必須符合法定對照品的質(zhì)量標(biāo)準(zhǔn)，或其他適用的質(zhì)量標(biāo)準(zhǔn)，且標(biāo)準(zhǔn)

28、偏差必須£ 2.0%。Assay: Prepare five solutions of the standard material under qualification according to the method for which it is to be used (two different analysts). Prepare the official RS or other qualified RS in the same manner. The results must comply with the official RS specification or othe

29、r applicable specifications and the standard deviation must be £ 2.0%.2.4.1.4.4有關(guān)物質(zhì)：按藥典方法或內(nèi)部方法進(jìn)行檢驗(yàn)。Related substance: Perform this test when available as a compendial monograph test or an in-house method.2.4.1.4.5水分：在標(biāo)準(zhǔn)品確認(rèn)時檢驗(yàn)。Water: Perform this test at the time of standard qualification.2.4.1.

30、4.6殘留溶劑：按藥典方法或內(nèi)部方法進(jìn)行檢驗(yàn)。Residual solvents: Perform this test when available as a compendial monograph test or an in-house method.2.5當(dāng)沒有法定對照品（如，USP、EP、CP等），或其他已確認(rèn)的對照品時，內(nèi)部使用的對照品的確認(rèn)。Qualification of an in-house reference standard when official reference standard (e.g., USP, EP, CP, etc.), or other quali

31、fied standard is not available.2.5.1起草一份對照品的確認(rèn)方案，方案包括下面的信息：Prepare a qualification protocol of reference standard, including the following information:2.5.1.1物料的鑒別，包括來源（如，生產(chǎn)廠家）以及批號。Identification of the material, including source (e.g., manufacturer) and lot number.責(zé) 任 人操 作RESPONSIBILITYACTION2.5.1.

32、2檢驗(yàn)報(bào)告書：結(jié)構(gòu)確證數(shù)據(jù)，如元素分析、NMR、MS、LC-MS、和IR；純度不低于98.0%；水分；殘留溶劑；有關(guān)物質(zhì)。如果這些沒有，則有關(guān)的檢驗(yàn)是必需的，檢驗(yàn)可以在公司內(nèi)完成，也可以在批準(zhǔn)的適當(dāng)?shù)墓就鈱?shí)驗(yàn)室完成。如果物料的含量低于98.0%，通過適當(dāng)?shù)臋z驗(yàn)，以及QC和QA的批準(zhǔn)，仍可以批準(zhǔn)為內(nèi)部使用的對照品（如，雜質(zhì)對照品的含量可低于98.0%）。如果物料為現(xiàn)有的原料，則必須符合所有適用的原料的質(zhì)量標(biāo)準(zhǔn)。Certificate of Analysis: Characterization data, e.g. Elemental Analysis, NMR, MS, LC-MS and I

33、R; a purity of at least 98.0%; water content; residual solvents; and related substance. If this is not available then the related testing is necessary and may be performed in-house or at an approved and appropriate laboratory. If the material is less than 98.0%, it may still be approved as an in-hou

34、se RS with appropriate testing and the approval of QC and QA (e.g., impurity RS may be < 98.0%). If the material is an existing raw material, it must meet all applicable raw material specifications.2.5.1.3檢驗(yàn)方法和結(jié)果：內(nèi)部使用的對照品的檢驗(yàn)通常必須包括其所使用時的方法。Methods of Analysis and Results: Testing of in-house refer

35、ence standard must always include the method for which it is to be used.2.5.1.3.1根據(jù)內(nèi)部使用的對照品所要用于檢驗(yàn)的，所適用的產(chǎn)品的方法中標(biāo)準(zhǔn)溶液的配制方法，對內(nèi)部使用的對照品進(jìn)行檢驗(yàn)。Test the proposed in-house reference standard according to the method for which it should be used by following only the standard preparation procedure in the applicabl

36、e product for the proposed in-house reference standard.責(zé) 任 人操 作RESPONSIBILITYACTION2.5.1.3.2線性：根據(jù)建議的對照品所要用于的方法，配制三個溶液。根據(jù)方法中所規(guī)定的范圍限度，配制高、中、低三個濃度的溶液。如果范圍沒有規(guī)定，則在目前水平的±15%配制。檢測儀器對所有溶液的三個讀數(shù)的響應(yīng)，按面積歸一化法計(jì)算。相關(guān)系數(shù)（r2）應(yīng)³ 0.995。Linearity: Prepare, in triplicate, three concentrations of the proposed sta

37、ndard material according to the method for which it is to be used. Prepare the solutions at the upper, mid and lower limit of the range specified in the method. If a range is not specified, prepare the solutions at ±15% of the target level. Measure instrument response for three readings of all

38、solutions and perform least squares fit analysis. The correlation coefficient (r2) should be ³ 0.995.2.5.1.3.3含量：根據(jù)所要用于的方法，配制五份待確認(rèn)對照品的溶液（雙人）。檢測儀器對溶液的響應(yīng)。結(jié)果必須符合質(zhì)量標(biāo)準(zhǔn)，且標(biāo)準(zhǔn)偏差£ 2.0%。Assay: Prepare five solutions of the standard material under qualification according to the method for which it is

39、to be used (two different analysts). Measure instrument response for the solutions. The results must comply with specifications with a standard deviation of £ 2.0%.2.5.1.4.4有關(guān)物質(zhì)：按生產(chǎn)廠家或內(nèi)部方法進(jìn)行檢驗(yàn)。Related substances: Perform this test when available as a manufacturers test or an in-house method.2.5

40、.1.4.5水分：在標(biāo)準(zhǔn)品確認(rèn)時檢驗(yàn)。Water: Perform this test at the time of standard qualification.2.5.1.4.6殘留溶劑：按生產(chǎn)廠家或內(nèi)部方法進(jìn)行檢驗(yàn)。Residual solvents: Perform this test when available as a manufacturers test or an in-house method.2.6對于由研發(fā)轉(zhuǎn)來的對照品For reference standards transferred from the R&D department.2.6.1研發(fā)部門應(yīng)提供相

41、應(yīng)的檢驗(yàn)報(bào)告書、圖譜，以及任何有關(guān)的文件，并提供該對照品的制備方法（若為自己合成）。R&D Department should provide the appropriate certificate of analysis, chromatogram, and any other related documents; and provide the synthesis process, if it is prepared in-house.責(zé) 任 人操 作RESPONSIBILITYACTIONQC2.6.2化驗(yàn)室接收后，根據(jù)上面的確認(rèn)要求，起草相應(yīng)的確認(rèn)方案進(jìn)行對照品的確認(rèn)。Afte

42、r receipt, QA should prepare the appropriate qualification protocol of the proposed reference standard according to the above qualification requirements.2.6對于雜質(zhì)對照品，根據(jù)雜質(zhì)對照品的性質(zhì)（如，定性的或定量的），根據(jù)上面的要求，制訂適當(dāng)?shù)拇_認(rèn)方案。For impurity standards, appropriate qualification protocol should be prepared according to the n

43、ature of impurity standards (such as qualitative or quantitative).3.評價(jià)、放行EVALUATION AND RELEASEQC, QA3.1確認(rèn)結(jié)束后，化驗(yàn)員將相關(guān)資料送QC主管審核，轉(zhuǎn)至QA進(jìn)行最終的評價(jià)、放行。Upon completion of the qualification, analyst forwards the related documents to QC Supervisor for review, then submit to QA for final review and release.3.1.1基

44、準(zhǔn)對照品Primary Reference Standard3.1.1.1一般純度應(yīng)大于99.0%。In general, Purity should ³ 99.0%.3.1.1.2純度大于99.0%的，視其含量為100.0%，直接參與計(jì)算。If the purity > 99.0%, the assay could be regarded as 100.0%, and could directly used in calculation.QA3.1.1.3已知雜質(zhì)、溶劑、水合物和無機(jī)鹽可能會使基準(zhǔn)對照品的純度小于99.0%，此時，基準(zhǔn)對照品的純度值應(yīng)按實(shí)際標(biāo)示，在樣品測定中應(yīng)

45、加以折算。Known impurities, residual solvents, hydrate, and abio-salt could make the purity < 99.0%, in such case, the purity of the primary reference standard should be marked with the actual value, and it should be converted in sample testing.3.1.2第二對照品Secondary Reference Standard3.1.2.1經(jīng)測得含量大于99.0%

46、的，純度為100.0%。If the assay > 99.0%, the purity could be regarded as 100.0%.3.1.2.2經(jīng)測定含量小于99.0%的，按實(shí)際純度值進(jìn)行折算。If assay < 99.0%, it should be converted based on the actual value.責(zé) 任 人操 作RESPONSIBILITYACTION3.2再確認(rèn)期和有效期Re-qualification data and Expiry date3.2.1再確認(rèn)期：在批準(zhǔn)后，給定一年的再確認(rèn)期。根據(jù)可利用的數(shù)據(jù)，給定在最初的再確認(rèn)期以后

47、的再確認(rèn)期。Re-qualification date: Upon approval, the reference standard should be assigned a one-year re-qualification date. Re-qualification date assigned after the initial re-qualification period should be established based on available data.3.2.1.1對于連續(xù)使用的，對照品必須在再確認(rèn)日期之前完成再確認(rèn)。For continued use, the stan

48、dard must be re-qualified prior to the re-qualification date.3.2.1.2采用與對照品最初批準(zhǔn)時相同的方法、標(biāo)準(zhǔn)，對含量、有效物質(zhì)和水分進(jìn)行檢驗(yàn)。Perform assay, related substances and water tests in the same manner and using the same criteria used for the initial standard approval.3.2.1.3對照品再確認(rèn)的日期按對照品接收之日，或生產(chǎn)日期（若為自己合成）計(jì)算，除非生產(chǎn)商或供應(yīng)商有規(guī)定的。The r

49、e-qualification date should be calculated on the date the RS received or manufactured (if it is prepared in-house), except it is specified by the manufacturer or supplier.注：如果對照品在再確認(rèn)時，不符合規(guī)定，則根據(jù)SOP3-0002進(jìn)行調(diào)查。Note: When a standard fails re-qualification, conduct an investigation according to SOP 3-000

50、2.3.2.2有效期：根據(jù)歷史數(shù)據(jù)，不穩(wěn)定的對照品應(yīng)給定有效期，超過有效期即不能再使用。Expiry date: Unstable standards should be assigned an expiry date, based on historical data, beyond which they may not be used.QA3.3檢驗(yàn)報(bào)告書Certificate of Analysis (COA)3.3.1對照品批準(zhǔn)后，QA出具檢驗(yàn)報(bào)告書，經(jīng)QA經(jīng)理簽字批準(zhǔn)后，予以放行使用。Upon approval, QA should issue COA, and

51、after approved by QA Manager, it could be released for use.3.3.2對照品的檢驗(yàn)報(bào)告書應(yīng)包括如下內(nèi)容，包括但不僅限于：The COA of the reference standard should include the followings, but is not limited to:3.3.2.1對照品的名稱、公司內(nèi)批號、類別。Reference standard name, in-house lot number, classification3.3.2.2供應(yīng)商的名稱、批號。Suppliers name, batch number責(zé) 任 人操 作RESPONSIBILITYACTION3.3.2.3檢驗(yàn)項(xiàng)目、標(biāo)準(zhǔn)規(guī)定、檢驗(yàn)結(jié)果。Test items, specification, test results3.3.2.4貯藏條件、使用說明。Storage condition, instruction for use3.3.2.5其他需說明的事項(xiàng)。Any other items to be specified3.3.3對照品檢驗(yàn)報(bào)告書號由：RS2位數(shù)年的年、月、日2位數(shù)的流水號組成。如“RS050908-01”表示為2005年9月8日簽發(fā)的第一份對照品檢驗(yàn)