【正文】 國際方法匯編 ）中且所參考的分析方法未經(jīng)過修改的話，則需提供該分析方法的參引，而不用提供該分析方法的描述（ 21 CFR ）。 分析方法描述中需要包括的典型內(nèi)容如下所示： A. Principle A statement of the principle of the analytical procedure should be included. For example, separation is based on isocratic reversed phase HPLC with detection by UV. B. Sampling The number of samples (., vials, tablets) selected, how they are used (., as individual or posite samples), and the number of replicate analyses per sample should be described. A．基本方法 HPLC進行分離的，檢測器為 UV 檢測器。 C. Equipment and Equipment Parameters A listing of all equipment (., instrument type, detector, column type, dimensions) should be included, as well as a list of equipment parameters (., flow rate, temperatures, run time, wavelength settings). A drawing representing the experimental configuration (., illustrating positions for a spray pattern analytical procedure) should be provided, when appropriate. C． 儀器和儀器參數(shù) 需要敘述的有：儀器列表（比如，儀器類型，檢測器，柱子類型，尺寸等）和儀器參數(shù)（比如，流速，溫度，運行時間和設(shè)定波長等）。 D. Reagents A list of reagents and their grades (., USP/NF, American Chemical Society (ACS) Analytical Reagent) should be included. If inhouse or modified mercial reagents are used, directions for their preparation should be included. Unstable or potentially hazardous reagents should be identified, and storage conditions, directions for safe use, and usable shelf life for these reagents should be specified. D． 試劑 需要敘述的有：試劑列表及其相應(yīng)的規(guī)格（比如： USP/NF，美國化學(xué)社（ ACS）分析試劑）。對于不穩(wěn)定的或有潛在危險的試劑，應(yīng)標明其儲存條件，安全使用說明和使用周期。系統(tǒng)適應(yīng)性實驗確保系統(tǒng)在樣品分析的時候能很好地運行。 All chromatographic analytical procedures should include system suitability testing and criteria. Parameters typically used in system suitability evaluations are defined and discussed in the CDER reviewer guidance on Validation of Chromatographic Methods (November 1994). 所有的色譜分析方法都應(yīng)當要有系統(tǒng)適應(yīng)性實驗及相應(yīng)的合格標準。 System suitability testing is remended as a ponent of any analytical procedure, not just those that involve chromatographic techniques. Regardless of the type of analytical procedure, testing should be used to confirm that the system will function correctly independent of the environmental conditions. For example, titration analytical procedures should always include the evaluation of a blank (monly referred to as a blank titration). 建議系統(tǒng)適應(yīng)性實驗應(yīng)成為所有分析方法的一部分，而不僅僅是色譜分析方法。比如說，滴定法一般來說需要進行空白實驗。 G. Preparation of Samples Sample preparation for individual tests should be clearly described. Specific details should be provided for unusual sample preparations (., solidphase extraction, derivatization). 應(yīng)當要按操作步驟對操作過程進行逐步敘述。需標明不常見的危險。所有用于數(shù)據(jù)分析的數(shù)學(xué)轉(zhuǎn)換或公式應(yīng)詳細描述。 of Results 1. General The format used to report results (., percent label claim, weight/weight, weight/volume, parts per million (ppm)) including the specific number of significant figures to be reported should be provided. 1． 通則 應(yīng)該規(guī)定關(guān)鍵計算步驟中的數(shù)字單位（例如， ‘ 標簽 ’ 標示量的百分比， W/W， W/L， ppm等） 2. Impurities Analytical Procedures The name and location/identifier (., retention time (RT), relative retention time (RRT)) of impurities and the type of impurity (., process, degradant, excipient degradant) should be included in the analytical procedures for impurities in the drug substance and drug product. The detection limit (DL) or quantitation limit (QL) should be stated, as appropriate. The DL or QL can be set using the drug substance39。也可以在原料藥檢測中設(shè)置 DL和 QL?？傆袡C雜質(zhì)是指所有達到或超過其自身定量限度的雜質(zhì)的總量。無機雜質(zhì)和溶劑的殘留，也應(yīng)該被提到。 The above reporting information may not be strictly applicable to all products (., biological, biotechnological, botanical, radiopharmaceutical drugs), but any significant process and productrelated impurities should be determined and reported. 并不是所有產(chǎn)品（比如，生物制劑、生物工藝制劑、植物制劑、放射制劑）的報告都必須嚴格按照以上談到的內(nèi)容來寫，但是所有關(guān)鍵的工序以及產(chǎn)品相關(guān)的雜質(zhì)都要有檢測和報告。 分析方法驗證 是個論述分析方法是適用于其擬定用途的過程。 The International Conference on Harmonisation (ICH) guidance Q2A Text on Validation of Analytical Procedures (March 1995) and Q2B Validation of Analytical Procedures: Methodology (November 1996) provide remendations on validation of analytical procedures. Analytical procedures outside the scope of the ICH guidances should still be validated. ICH指導(dǎo)原則 Q2A：分析方法驗證（ 1995年 3月）和 Q2B：分析方法驗證：方法學(xué)（ 1996年11 月）給出了分析方法驗證的建議。 1. Validation Characteristics Applicants should submit information on the validation characteristics of their proposed analytical procedures (see ICH Q2A and ICH Q2B). Although not all of the validation characteristics are needed for all types of tests (see section ), typical validation characteristics are: 申請者應(yīng)當要送交其所擬定分析方法的驗證項目方面的信息（見 ICH Q2A和 ICH Q2B）。 Legible reproductions of representative instrument output or recordings (., chromatograms) and raw data output (., integrated areas), as appropriate. Instrument output for placebo, standard, and sample should also be provided (see section ). 清晰可讀的儀器代表性輸出和記錄資料（如色譜圖）和原始資料輸出（積分面積）。 Representative calculations using submitted raw data, to show how the impurities in drug substance are calculated. Information from stress studies (see section ). Impurities labeled with their names and location identifiers (., RRT for chromatographic data) for the impurity analytical procedure. 代表性計算公式，以表明原料藥中的雜質(zhì)是如何計算的。對于雜質(zhì)分析方法，要標明雜質(zhì)的名稱和位置標識符（如，色譜中的相對保留時間 RRT）。 對每個有機雜質(zhì)進行適當?shù)臉俗R和界定。對于其它雜質(zhì)（如無機雜質(zhì)，殘留溶劑），應(yīng)當要進行說明并定量分析。 已知雜質(zhì)列表，包括工藝雜質(zhì)，降解產(chǎn)物和可能的異構(gòu)體。 For drug products: A degradation pathway for the drug substance in the dosage form, 419where possible. Data demonstrating recovery from the sample matrix as illustrated by the accuracy studies. Data demonstrating that neither the freshly prepared nor the degraded placebo interferes with the quantitation of the active ingredient. ICH Q2A and Q2B address almost all of the validation parameters. Areas that should be provided in more detail are described below. 對于制劑： 原料藥在制劑中可能的降解途徑。要有資料論證無論是新制的安慰劑還是分解了的安慰劑都不會影響活性成分的定量分析。下面論述的是那些還需要更詳細地進行論述的方