分析方法驗(yàn)證程序

1、分析方法驗(yàn)證程序 SOP 審核和批準(zhǔn) SOP Review and Approval 1.0 2.0 3.0 目的 Purpose 本規(guī)程的目的是為在 XXX 有限公司進(jìn)行的驗(yàn)證研究制定一個(gè)程序，包括分析方法驗(yàn)證 過(guò)程，分析方法的確認(rèn)，文件記錄，審計(jì)，原始數(shù)據(jù)歸檔以及驗(yàn)證 / 確認(rèn)文件放行。 范圍 Scope 2.1 本標(biāo)準(zhǔn)操作程序適用于 XXX有限公司產(chǎn)品研發(fā)部門(mén) GMP分析實(shí)驗(yàn)室， 采用色譜技術(shù)對(duì)最終成品和 API （如適用）進(jìn)行的所有分析方法的驗(yàn)證 / 確認(rèn)。 2.2 本標(biāo)準(zhǔn)操作程序也可作為 XXX 有限公司產(chǎn)品研發(fā)部門(mén)分析研發(fā)實(shí)驗(yàn)室， 采用其他分析技術(shù)進(jìn)行其他任何方法驗(yàn)證 / 確認(rèn)的參

2、考。 c. 職責(zé) Responsibility 3.1 分析員 Analyst 3.1.1 負(fù)責(zé)準(zhǔn)備驗(yàn)證方案 3.1.2 / of method validation / method 3.1.3 / 確認(rèn)報(bào)告 Responsible for preparation of method validation report / method verification report 3.2 4.0 主管小組 / 指定人員 Group In-charge/ Designee 3.2.1 負(fù)責(zé)復(fù)核和審批驗(yàn)證方案 Responsible for review & approval of validati

3、on protocol 3.2.2 負(fù)責(zé)方法驗(yàn)證 / 確認(rèn)活動(dòng)的分配、監(jiān)督以及驗(yàn)證 / 確認(rèn)數(shù)據(jù)的復(fù) 核 Responsible for allotment & monitoring of method validation / verification activity and review of validation / verification data 3.2.3 負(fù)責(zé)驗(yàn)證報(bào)告 / 確認(rèn)報(bào)告的復(fù)核和審批 Responsible for review & approval of validation report / verification report 3.3 質(zhì)量保證 Qualit

4、y Assurance 3.3.1 負(fù)責(zé)驗(yàn)證報(bào)告 / 確認(rèn)方案的復(fù)核和審批 protocol 3.3.2 負(fù)責(zé)驗(yàn)證報(bào)告 / report 3.4 注冊(cè) Regulatory 3.4.1 負(fù)驗(yàn) / 案的復(fù)核 Responsible for review of 簡(jiǎn)寫(xiě)和定義 為了啟動(dòng)方法驗(yàn)證，相關(guān)人員或者指定人員應(yīng)該起草驗(yàn)證方案。驗(yàn)證方案應(yīng)該包含在 驗(yàn)證過(guò)程中所有需要研究的參數(shù)和接受標(biāo)準(zhǔn)。相關(guān)主管或者指定人員應(yīng)該對(duì)驗(yàn)證方案進(jìn)行 復(fù)核。 To initiate method validation, a validation protocol should be filled by the concer

5、ned person / designee. The validation protocol should contain all the parameters required to be studied during the validation along with acceptance criteria. Validation protocol should be checked by the concerned group head / designee. 備注：對(duì)于方法確認(rèn)，不要求準(zhǔn)備方案。 Note:There is no requirement to prepare any p

6、rotocol for method verification activity. 驗(yàn)證方案應(yīng)該有 QA 給定的唯一編號(hào)。 The validation protocol should have a unique number given to it by the quality assurance. 5.1 5.2 5.3 5.4 5.5 QA 和注冊(cè)(如適用)批準(zhǔn)。 charge /designee followed by a representative of QA& Regulatory (if applicable). / 觀 pH 測(cè)定)。 Validation be record

7、ed in laboratory note book (dedicated for validation only) against each approved validation notebook.Verification is not required for basic compendial test procedures that are routinely performed (e.g. loss on drying, residue on ignition, various wet chemical procedures such as acid value, and simpl

8、e instrumental determinations such as pH measurements). 在實(shí)驗(yàn)進(jìn)行過(guò)程中或者實(shí)驗(yàn)完成后，來(lái)自方案的任何偏差應(yīng)該被評(píng)估。任何來(lái)自方案 的增補(bǔ)或變更應(yīng)該在驗(yàn)證方案的合適章節(jié)中提到。 During the execution of experimental work or after its completion, any deviation from the protocol should be justified. Any additions or changes from the protocol should be mentioned

9、under appropriate section in validation protocol. 如果在之后的時(shí)間里，發(fā)現(xiàn)批準(zhǔn)的方案中有一些小的差異或錯(cuò)誤，如印刷或輸入錯(cuò)誤， 主管或指定人員應(yīng)該用“勘誤表”說(shuō)明并糾正這些錯(cuò)誤。If at a later date minor discrepancies or errors are noticed in the approved validation protocol, such as typographical and transcriptional errors, an 5.6 ERRATUM stating these errors, a

10、long with the correction, should be prepared by the group in-charge/designee. 5.7 在驗(yàn)證研究過(guò)程中，如果需要做額外的一些實(shí)驗(yàn) / 參數(shù)，但它們不是主驗(yàn)證方案的一 部分，就需要再產(chǎn)生一個(gè)補(bǔ)充方案（以及相應(yīng)的編號(hào)），補(bǔ)充的實(shí)驗(yàn)將成為驗(yàn)證報(bào)告的一 部分。 During the course of validation studies, if any additional experiment / parameter needs to be done which is not part of the main valid

11、ation protocol, an addendum protocol （and corresponding number） need to be taken, if that additional experiment will be part of validation report. 備注：補(bǔ)充驗(yàn)證方案可在最終的驗(yàn)證報(bào)告批準(zhǔn)前的任何時(shí)間產(chǎn)生。最終的驗(yàn)證報(bào)告應(yīng) 包括來(lái)自于主驗(yàn)證方案和補(bǔ)充驗(yàn)證方案 （如果有 ） 的數(shù)據(jù)。 Note: Addendum validation protocol can be taken any time before the approval of final

12、 validation report. The final validation report should include the data generated against the main validation protocol and addendum 5.9 單個(gè)驗(yàn)證方案中的接受標(biāo)準(zhǔn)可參考附件 -A 中規(guī)定的接受標(biāo)準(zhǔn)，最終在批 準(zhǔn)的驗(yàn)證方案中的規(guī)定接受標(biāo)準(zhǔn)將會(huì)取代SOP中規(guī)定的接受標(biāo)準(zhǔn)。 The acceptance criteria specified in appendix-A can be used as reference to define the acceptance

13、criteria in the individual validation protocol. Finally, the acceptance criteria specified in approved validation protocol will supersedes the acceptance criteria specified in this standard operating procedure. 5.10 在實(shí)驗(yàn)工作和計(jì)算完成后，分析員應(yīng)該準(zhǔn)備驗(yàn)證 / 確認(rèn)報(bào)告草案。 On completion of the experimental work and calculati

14、ons, a draft validation report/ verification report should be prepared by analyst. 5.11 主管/ 指定人員以及之后的 QA ，應(yīng)該從準(zhǔn)確度和完整性角度審核驗(yàn)證/ 確 認(rèn)報(bào)告草案和方法驗(yàn)證研究的原始記錄。 The draft validation report / verification report and the raw data of the method validation studies should be reviewed for accuracy and adequacy by group-i

15、n-charge / designee, followed by quality assurance. 5.12 告。 5.13 分析部門(mén)主管 /QA/ 指定人員審批。 報(bào)告應(yīng)該有 QA The report should by Head Analytical Research (or R&D) / Designee, Assurance / Designee. The validation report 5.14 The final copy of the report along with the raw data should be archived. The draft reports

16、hould not be retained. 5.15 如果在最終報(bào)告簽署后，要求產(chǎn)生額外的數(shù)據(jù)而不是更新原來(lái)已經(jīng)存在 的數(shù)據(jù)，應(yīng)進(jìn)行額外的實(shí)驗(yàn)工作，并準(zhǔn)備一份原報(bào)告附錄，放行額外產(chǎn)生的數(shù)據(jù)。 If at a later date additional data other than the already existing data is required to be generated, additional experimental work should be carried out and an addendum to the original validation report s

17、hould be prepared and issued. 5.16 如果報(bào)告批準(zhǔn)后，發(fā)現(xiàn)一些小的差異和錯(cuò)誤，如印刷或輸入錯(cuò)誤(不超 5 個(gè)或 過(guò) 5 個(gè))，應(yīng)準(zhǔn)備“勘誤表”說(shuō)明和糾正這些錯(cuò)誤。如果印刷或輸入錯(cuò)誤超過(guò) 者需要對(duì)一些現(xiàn)存數(shù)據(jù)的報(bào)告進(jìn)行修正，那就需要準(zhǔn)備和放行修訂版本的報(bào)告或者補(bǔ)充報(bào) 告。 If at a later date minor discrepancies or errors are noticed in the approved reportreport, such as typographical and transcriptional errors (not mor

18、e than five in number), an ERRATA stating these errors, along with the correction, should be prepared. If the typographical and transcriptional errors are more than five or there is any modification in the reporting of an existing data, a revised v report or addendum report should be prepared and is

19、sued. 5.17 原報(bào)告修訂的原因應(yīng)該清晰地在修訂的報(bào)告中闡述。修訂報(bào)告和原始記 錄應(yīng)該交給 QA 審計(jì)。 The reason for revision of the original report should be clearly stated in the introduction of the revised report. The revised validation report and the raw data should be submitted to quality assurance for audit. 5.18 批準(zhǔn)的報(bào)告，以及原始記錄、補(bǔ)充文件、勘誤表和升級(jí)版本，都應(yīng)該歸