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WHO驗證指南:分析方法驗證-英譯中


南京翻譯公司英譯中文件---APPENDIX 4  ANALYTICAL METHOD VALIDATION

分析方法驗證

1. Principle

原則

2. General

常規

3. Pharmacopoeial methods

藥典方法

4. Non-pharmacopoeial methods

非藥典方法

5. Method validation

方法驗證

6. Method verification

方法確認

7. Method transfer

方法轉移

8. Revalidation

再驗證

9. Characteristics of analytical procedures

分析方法的特征

 

1. PRINCIPLE

原則

 

1.1 This appendix presents some information on the characteristics that should be considered during validation of analytical methods. Approaches other than those specified in this appendix may be followed and may be acceptable. Manufacturers should choose the validation protocol  and procedures most suitable for testing of their product.

本附錄給出了一些分析方法驗證過程中中需要考慮的特性信息。除了在附錄里指定的方法以外,其它方法也可以采用。 廠家應選擇適合自身樣品檢驗的驗證方案和程序。

1.2 The manufacturer should demonstrate (through validation) that the analytical procedure is  suitable for its intended purpose.

廠家應當證明(通過驗證)分析的程序是符合預期目的的

1.3 Analytical methods, whether or not they indicate stability, should be validated.

分析方法是否穩定,都應該被驗證

1.4 The analytical method should be validated by research and development before being transferred to the quality control unit when appropriate.

適當時,分析方法在轉移給質量控制部門之前, 需要在研發進行驗證

1.5 The recommendations as provided for in good laboratory practices and guidelines for transfer of technology should be considered, where applicable, when analytical method validation is organized and planned.

如適用,在組織和計劃方法驗證時, GLP和技術轉移指南所推薦的條目應該被考慮

 

2. GENERAL

一般原則

 

2.1 There should be specifications for both materials and products. The tests to be performed should be described in the documentation on standard test methods

原料和成品的分析方法應該有規范, 需要執行的分析應該在文件中描述標準的測試方法

2.2 Specifications and standard test methods in pharmacopoeias (“pharmacopoeial methods”), or suitably developed specifications or test methods (“non-pharmacopoeial methods”) as approved by the national regulatory authority (NRA) may be used.

可以使用藥典中規定的規范和標準測試方法(藥典方法)或者經過適當開發的經國家藥品監督管理部門認可的規范或方法(非藥典方法) 

2.3 Well-characterized reference materials, with documented purity, should be used in analysis. 

應該在分析中使用具有文件證明其純度的特定對照物

2.4 The most common analytical procedures include identification tests, assay of drug substances and pharmaceutical products, quantitative tests for content of impurities and limit tests for impurities. Other analytical procedures include dissolution testing and determination of particle size. 

常見的分析程序包括鑒別、含量、雜質定量測試和雜質限度,其他分析程序還包括溶出度和粒徑測定

2.5 The results of analytical procedures should be accurate, legible, contemporaneous, original, reliable and reproducible. All results should be archived for an appropriate period of time as defined by the laboratory and be in compliance with NRA requirements.

檢驗的結果應精確,清晰,同步,原始,可靠,并可再現。所有結果應該按照實驗室定義的時間周期妥善保存并符合國家監管要求。

2.6 The procedure should become part of a continuous verification procedure to demonstrate that it meets the predefined criteria over the life of the procedure. 

該程序應成為持續確認程序的一部分,以證實它在其生命周期內符合既定的標準。

2.7 Trend analysis and risk assessment should be considered at intervals to ensure that the method is appropriate for its intended application. 

應該考慮定期進行趨勢分析和風險評估以確保該分析方法符合其預期用途

2.8 Changes to methods should be managed in accordance with the authorized change control procedure. The variability of reference materials and other factors such as changes in the process for synthesis of the drug substance, changes in the composition of the finished product, changes in the analytical procedure, when analytical methods are transferred from one laboratory to another (when method transfer is not possible) or when major pieces of equipment instruments change should be considered. These should be understood, controlled and, where possible, reduced. Verification or revalidation should be considered where appropriate.

分析方法的變更應該按照批準的變更管理規程進行管理。當分析方法從一個實驗室轉移到另一個或當主要設備儀器變化時應考慮對照物的可變性以及其他因素如藥品合成工藝的變化,藥品組分的變化,分析程序的變化。這些應該被理解,控制和適當的減少。適當時,應該考慮進行確認或再驗證。

2.9 The scope of verification or degree of revalidation depend on the nature of the change(s) and the outcome of risk assessment.

驗證的范圍或再驗證的程度取決于變更的性質和風險評估的結果

2.10 There should be evidence that the analysts, who are responsible for certain tests, are appropriately qualified to perform those analyses (“analyst proficiency”).

應有證據表明負責某一測試的分析師應該被確認可以執行該測試(分析熟練程度)

2.11 The data obtained during method validation and verification should be considered covered by good anything practices (GxP) requirements and are expected to follow the principles of good data and record management practices (2). Their associated metadata are also expected to be retained and subjected to good data and record management practices.

在分析方法驗證和方法分析方法驗證和確認過程中獲得的數據應符合GXP的要求和遵循良好數據和記錄管理規范的要求。它們的元數據也應該被保存并符合良好數據和記錄管理規范要求。

2.12 When computerized systems are used to obtain and process data relating to method validation and verification, they should comply to the principles enunciated in Appendix 5 – Validation of computerized systems.

當使用計算機化系統獲取和處理方法驗證和確認相關的數據時,應該遵循附錄5—計算機化系統驗證的原則。 

2.13 Adequate attention should be paid to the method of sample preparation. The description of this step should be as detailed as possible, especially if it can have a significant impact on tests results (e.g. particular attention should be paid to details such as sonication time, sonication bath temperature and mixing and to samples where demixing is known to occur).

應該充分重視樣品處理的方法,對這一步驟的描述應盡可能的詳細,特別是當它對檢測結果有重要影響時(例如應該特別重視如超聲時間,超聲池溫度和攪拌和當已知會分層時進行取樣等細節)

2.14 Failures occurring during method validation, and how these were overcome, should be included in the method validation report – it is not acceptable to present only the passing results as it will give a biased imaged on the reliability of the method and on how it should be applied.

方法驗證過程中發生的失敗,以及如何處理這些失敗的,應該包括在方法驗證報告中。僅僅包括合格的結果是不接受的,因為他會對方法的可靠性和如何應該該方法產生偏頗。

 

3. PHARMACOPOEIAL METHODS

藥典方法

 

3.1 When pharmacopoeial methods are used, evidence should be available to prove that such methods are suitable for routine use in the laboratory (verification).

當使用藥典的方法時,要有證據證明這種方法在該實驗室日常使用是適用的。

3.2 Pharmacopoeial methods used for determination of content or impurities in pharmaceutical products should also have been demonstrated to be specific with respect to the substance under consideration (no placebo interference).

用于測定制劑產品中含量或雜質的藥典方法均應被證明在有主含量成分存在時具有專屬性(無空白干擾)。

 

4. NON-PHARMACOPOEIAL METHODS

非藥典方法

 

4.1 Non-pharmacopoeial methods should be appropriately validated.

非藥典方法應進行適當的驗證

 

5. METHOD VALIDATION

方法驗證

 

5.1 Validation should be performed in accordance with the validation protocol. The protocol should include procedures and acceptance criteria for all characteristics. The results should be documented in the validation report.

驗證應當按照預定的驗證方案進行,方案應該包括所有特性的驗證程序和接受標準,結果應當記錄在驗證報告中。

5.2 Justification should be provided when non-pharmacopoeial methods are used if pharmacopoeial methods are available. Justification should include data such as comparisons with the pharmacopoeial or other methods.

如果存在藥典方法可用,而使用了非藥典方法,則需要提供論證。論證應包括數據,例如與藥典或其它方法的比較。

5.3 Standard test methods should be described in detail and should provide sufficient information to allow properly trained analysts to perform the analysis in a reliable manner. As a minimum, the description should include the chromatographic conditions (in the case of chromatographic tests), reagents needed, reference standards, the formulae for the calculation of results and system suitability tests.

標準檢測方法應詳細描述,并提供充分的信息使得經過適當培訓的化驗員可以用可靠的方式進行分析。至少,描述應包括色譜條件(如果采用色譜測試),所需溶劑、標準對照品、結果計算公式和系統適用性檢測。

 

6. METHOD VERIFICATION

方法確認

 

6.1 Method verification consists of partial validation. It should be performed for already validated analytical methods under the following circumstances: (a) when an already validated method is used on a product for the first time (e.g. in case of a change in active pharmaceutical ingredient (API) supplier, change in the method of synthesis or after reformulation of a drug product); (b) when an already validated method is used for the first time in a laboratory (in some cases, method transfer may be preferable).

方法確認包含方法驗證的一部分,方法確認是針對已經驗證過的方法的以下幾種情形:(a)當使用一個驗證過的方法進行首次對一個產品進行檢測時,(例如:在API的供應商變更時,或者API合成方法變更或成品重新配方后)(b)方法第一次在一個實驗室使用時(在某些情況下,方法轉移更合意)

6.2 Method verification may include only the validation characteristics of relevance to the particular change. For instance, in the case of a change in API supplier, the only expected difference would be in the impurity profile or solubility of the API, and therefore, for a related substances method, there should be an appropriate verification that the method is able to detect and quantitate all potential impurities, even the late eluting ones. Specificity should be among the tests considered (see sections 9 and 10 below for more detail). 

方法確認可能只是驗證方法驗證中最容易受影響的那一部分,例如通過API供應商的改變,來改變雜質的分布或者API的溶解度,因此對于一個檢測方法,必須要進行適當的確認以確保該方法可以檢測出該樣品所有潛在的雜質甚至洗脫出的雜質,方法的特異性也是需要考慮的(第9和第10部分關于特異性會有更多的講解)

 

6.3 Method verification is suitable in lieu of method validation for pharmacopoeial methods.

方法確認適用于對藥典方法的驗證

 

7. METHOD REVALIDATION

方法再驗證

 

7.1 Methods should be maintained in a validated state over the life of the method (see point 2.6 above). Revalidation of an analytical procedure should be considered whenever there are changes made to the method, including: 

方法應在其生命周期內保持驗證狀態(見上述2.6),當方法發生變更時,應考慮進行再驗證,包括但不僅限于以下幾個方面:

 

 ‒ changes to the mobile phase (please refer to The International Pharmacopoeia and other pharmacopoeias for the acceptance limits beyond which revalidation must be performed);

流動相變更(請參考國際藥典和其它藥典關于一定要再驗證的可接受限度)

 ‒ changes to the column;

色譜柱變更

 ‒ changes to the temperature of the column;

柱溫變更

 ‒ changes to the concentration/composition of the sample and standards;

樣品和標準品濃度/成分變更

 ‒ changes to the detector (change in detector type, e.g. if going from ultraviolet (UV)- visible detection to fluorimetry, or wavelength of detection).

檢測器的變更(檢測器類型的變更,如,從紫外可見檢測變更為熒光檢測或波長檢測)

7.2 In case of repeated system suitability failures or when obtaining of doubtful results. In such cases an investigation of the root cause should be performed, the appropriate changes made and the method revalidated.

當重復的系統適應性失敗或得到可疑結果時,應進行根本原因調查,適當的變更以及方法再驗證。

7.3 Periodic revalidation of analytical methods should be considered according to a period that is scientifically justifiable.

應考慮分析方法的周期性再驗證,驗證的周期應進行科學的論證。

7.4 It is acceptable for revalidation to include only the validation characteristics of relevance to the particular change and method. 

再驗證時只包括某一變更和方法相關的驗證特性是可接受的。

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