【正文】 on and Accuracy 精密度和準確度 A minimum of 5 recovery determinations at each of 5 calibration levels must be 5個校準水平下必須每個水平至少測定 5個加標回收樣品 One set of recovery determinations must include a blank, and 5 or more nonzero spikes, including the LOQ as the low level.每組加標樣品必須包括空白、 5個以上非零加標，其中低值應為 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，以及精密度和準確度。 Intrabatch (withinbatch) accuracy and interbatch (between batch) accuracy may be pared as a measure of robustness.批內和批間準確度可認為是方法穩(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。 2 2 Taylor, . “Validation of Analytical Methods” (1983) Anal. Chem. 55, 600A608A 6 來自 中國最大的數(shù)據(jù)庫下載 ISO 17025: Validation is the confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are 法確認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 3 ISO 17025 Standard, element 7 來自 中國最大的數(shù)據(jù)庫下載 Objective of Method Validation 方法確認的目標 應具有 合理設計的 , 充分研究的 , 形成完整文件的 分析方法 能為 既定領域 提供 有用的數(shù)據(jù) To have properly designed, adequately studied, well documented analytical methods capable of producing useful data for the intended application 8 來自 中國最大的數(shù)據(jù)庫下載 Sequence of Events 方法確認工作的順序 : The process is not necessarily linear – it may be necessary to cycle back through method development at least once before the method can be successfully validated. 方法確認不一定是直線進程 – 它可能需要隨著方法的開發(fā)至少重復一次直到方法成功確認 . Method Development 方法改進 Method Validation 方法確認 Method Implementation 方法執(zhí)行 9 來自 中國最大的數(shù)據(jù)庫下載 General Classification of Method Validation Studies方法確認的分類 Interlaboratory (between laboratories)實驗室間 ? At least two independent laboratories involved至少兩個獨立實驗室 ? Sponsored by professional anizations (AOAC, ASTM)由專業(yè)組織承辦 ? AOAC Official Methods官方方法 – at least 8 labs至少8個實驗室 ? AOAC Peer Verified Methods同行驗證方法 – at least 2 labs至少 2個實驗室 Intralaboratory (within a laboratory)實驗室內 10 來自 中國最大的數(shù)據(jù)庫下載 Benefits of Method Validation 方法確認的益處 Assessment and optimization of method performance方法性能的評價和優(yōu)化 Generation of baseline data for parison to longterm QC data生成基準數(shù)據(jù)與長期的質控數(shù)據(jù)進行比較 Identification of instruments, other equipment, supplies and chemicals required識別分析儀器、其它設備、耗材和化學品的需求 ? Assessment of purchasing needs, cost and potential suppliers評價購買需求、價格和可能的供應商 11 來自 中國最大的數(shù)據(jù)庫下載 Benefits of Method Validation 方法確認的益處 Identification of personnel needs個人需求的識別 ? Expertise and training專業(yè)技能和培訓 Consideration of safety and hazardous waste disposal issues對實驗安全和有害廢物處理的考慮 Demonstration of the laboratory’s ability to meet the requirements of the customer實驗室對消費者需求的滿足能力的展示 12 來自 中國最大的數(shù)據(jù)庫下載 Benefits of Method Validation 方法確認的益處 Operational efficiency when method is implemented方法執(zhí)行后的操作效率 Design of QA/QC strategy QA/QC方案設計 Avoid embarrassment and damage to lab’s credibility when the method is implemented避免方法執(zhí)行后造成的對實驗室信譽的不良影響 Allows initial estimation of measurement uncertainty對測量不確定度進行初步評估 13 來自 中國最大的數(shù)據(jù)庫下載 When is Method Validation Necessary何時需要方法確認 ? Official methods (eg. USP, AOAC, Health Canada Compendium, etc.) do not require full internal validation, however the laboratory must官方方法不需要完整內部確認，不過實驗室必須 : ? Have procedures to demonstrate that the method is performing in the particular laboratory environment有程序證明在特定實驗室環(huán)境下該方法可行 . ? Retain