【導(dǎo)讀】來自中國最大的數(shù)據(jù)庫。ableto通過學(xué)習(xí)你將能夠:. 取相關(guān)確認(rèn)數(shù)據(jù)，對新方法進行評估。評價確認(rèn)數(shù)據(jù)，以確定方法確認(rèn)應(yīng)滿足的特。定要求已經(jīng)驗證并可接受。出限定量限,精密度,準(zhǔn)確度,不確定度。完整描述分析人員為獲得所需要的分析結(jié)。法確認(rèn)是通過檢查和提供客觀證據(jù)確證某。一特定用途的特殊要求已得到滿足3. 能為既定領(lǐng)域提供有用。方法確認(rèn)不一定是直線進程–它可能需要隨著方法的開發(fā)至。少重復(fù)一次直到方法成功確認(rèn).ASTM)由專業(yè)組織承辦。2labs至少2個實驗室。performance方法性能的評價和優(yōu)化。long-termQCdata生成基準(zhǔn)數(shù)據(jù)與長期的質(zhì)控數(shù)。其它設(shè)備、耗材和化學(xué)品的需求。suppliers評價購買需求、價格和可能的供應(yīng)商。disposalissues對實驗安全和有害廢物處理的考

　　

【正文】 ade that the spiked sample is chemically and physically representative of the actual samples加標(biāo)樣品在理化性質(zhì)上假設(shè)與實際樣品相同 Spike recovery data do not necessarily reveal the true recovery of the analyte from the sample加標(biāo)回收數(shù)據(jù)不必反映樣品被測物的實際回收率 51 來自 中國最大的數(shù)據(jù)庫下載 Precision and Accuracy 精密度和準(zhǔn)確度 A minimum of 5 recovery determinations at each of 5 calibration levels must be 5個校準(zhǔn)水平下必須每個水平至少測定 5個加標(biāo)回收樣品 One set of recovery determinations must include a blank, and 5 or more nonzero spikes, including the LOQ as the low level.每組加標(biāo)樣品必須包括空白、 5個以上非零加標(biāo)，其中低值應(yīng)為 LOQ 52 來自 中國最大的數(shù)據(jù)庫下載 Precision and Accuracy 精密度和準(zhǔn)確度 The linear range of the method, as well as precision and accuracy are calculated from these 到方法線性范圍，以及精密度和準(zhǔn)確度。 Intrabatch (withinbatch) accuracy and interbatch (between batch) accuracy may be pared as a measure of robustness.批內(nèi)和批間準(zhǔn)確度可認(rèn)為是方法穩(wěn)健度的測定 53 來自 中國最大的數(shù)據(jù)庫下載 Accuracy 準(zhǔn)確度 The accuracy required for a particular method may be specified in the reference method or by the 度可由顧客或參考方法規(guī)定 Alternatively, the acceptable range may be calculated from the method validation data.另外，可接受的測量范圍可通過方法確認(rèn)數(shù)據(jù)計算獲得 54 來自 中國最大的數(shù)據(jù)庫下載 Precision精密度 Precision精密度 : the closeness of agreement between a series of measurements一組測量值的接近程度 Precision includes both repeatability (same analyst and operating conditions over a short period of time) and reproducibility (different analyst, days, and/or operating conditions。 may also refer to precision between different laboratories)精密度包括重復(fù)性（短時間內(nèi)同一操作人員及相同條件下）和復(fù)現(xiàn)性（不同分析人員、不同工作日、不同操作條件、多指不同實驗室間的精密度） 55 來自 中國最大的數(shù)據(jù)庫下載 Precision精密度 Precision is expressed at each calibration level by calculating the %CV (standard deviation / mean value) x 100在每一校準(zhǔn)水平下精密度通過相對標(biāo)準(zhǔn)偏差計算得到 The required level of precision may be specified in the reference method or by the customer所需的精密度水平可在參考方法中或顧客規(guī)定 Typically, acceptable precision is less than 15% CV (20 % at the LOQ)一般 CV小于 15% (LOQ水平為 20 % ) 56 來自 中國最大的數(shù)據(jù)庫下載 Robustness Testing 穩(wěn)健度試驗 Examination of the behavior of an analytical process when small changes in the environment or operating conditions are made在環(huán)境或操作條件小的改變下，對分析過程的表現(xiàn)的檢查 57 來自 中國最大的數(shù)據(jù)庫下載 Benefits of Robustness Testing 穩(wěn)健度試驗的益處 Identification of critical control points關(guān)鍵控制點的識別 Ability to specify limits or restrictions for procedural steps in the method方法中各步驟某些限制的特殊規(guī)定 More effective and efficient implementation of the method in the laboratory 在實驗室執(zhí)行方法時更加有效 Example batch layout 58 來自 中國最大的數(shù)據(jù)庫下載 Validation Summary File 方法確認(rèn)總結(jié)文件 Method validation data must be summarized into a report that is clear and easy to 法確認(rèn)數(shù)據(jù)必須總結(jié)為清晰和易于執(zhí)行的報告 The summary must include總結(jié)中必須包括 : ? Sample type that was used with as much detail as possible (. tissue type and species)樣品類型，應(yīng)提供盡可能多的信息（如組織類型和種類） ? Statement of LOD, LOQ, Precision, Accuracy linearity對檢出限、定量限、精密度、準(zhǔn)確度和線性范圍的陳述 59 來自 中國最大的數(shù)據(jù)庫下載 Verification of Data 數(shù)據(jù)的驗證 Performed by QA 由 QA完成 Confirm a sampling of calculations (square root of total number。 double sample size if errors are found)從計算中抽取部分計算確證（總量的平方根，若發(fā)現(xiàn)錯誤，樣品量加倍） Inspect peak integration檢查峰的積分 Confirm sequence integrity確定順序的完整性 60 來自 中國最大的數(shù)據(jù)庫下載 Method SOP 方法標(biāo)準(zhǔn)操作程序 Once the validation data has been verified, a method SOP must be written for the procedure.一旦確認(rèn)數(shù)據(jù)通過驗證，實驗過程必須寫成方法標(biāo)準(zhǔn)操作程序 Include the validation data in the SOP, and specify acceptable ranges for precision and accuracy based on this data (must be at least as good as the reference method)方法標(biāo)準(zhǔn)操作程序中包括確認(rèn)數(shù)據(jù)，根據(jù)以上數(shù)據(jù)，規(guī)定在一可接受范圍內(nèi)的準(zhǔn)確度和精密度（必須至少要與參考方法相當(dāng)） 61 來自 中國最大的數(shù)據(jù)庫下載 Method Validation – Summary 方法確認(rèn) 總結(jié) Nonstandard methods must be validated in order to ply with ISO 17025非標(biāo)方法必須經(jīng)過確認(rèn)以符合 ISO 17025 Validation involves determination of several parameters, including LOD, LOQ, accuracy and precision方法確認(rèn)須測定若干參數(shù)包括 LOD、 LOQ、準(zhǔn)確度和精密度 Validation data must be summarized into a report and verified by QA確認(rèn)用數(shù)據(jù)必須編寫成報告并經(jīng) QA部門核查 Once verified, a method SOP must be writte驗證后，必須寫成方法標(biāo)準(zhǔn)操作程序