质量控制概要-PHPppt课件

1、 Review of Quality Control质量控制概要We will cover(内容)Terminology术语Characteristics of Analytical Methods分析方法特性Types of QC samples and how they relate to the characteristicsQC样品类型和特性.Definition of Quality质量的定义To most of the world (普遍上) degree of excellence(优良程度)To the ISO world (在ISO领域) degree of agreemen

2、t between characteristics and requirements特性与要求的吻合程度More importantly (更重要) to our clients?(对客户).Quality Control vs. Quality Assurance(质量控制与质量保证)Quality control is a series of measurements used to assess the quality of the analytical data质量控制是一系列丈量,以评价分析数据的质量How well is the test fulfilling requiremen

3、ts?实验满足要求的程度如何?.Quality Control vs. Quality Assurance (质量控制与质量保证)Quality assurance is a management plan to ensure the integrity of data (a system)质量保证是一种管理方案,以确保数据的完好性(一种体系)Provides confidence that requirements will be fulfilled为要求能否得到满足提供自信心.Qualities of Analytical Methods分析方法的质量Accuracy(准确度)Precis

4、ion(精细度)Selectivity(选择性)Sensitivity(灵敏度)Linearity(线性)Range(范围)Robustness / Ruggedness(稳健性/稳度).Accuracy(准确度)Degree of agreement between the “true value and the measured value(真值与丈量值之间的一致程度).Accuracy (准确度)What is the “true value?(什么是真值)Theoretical(实际值)Consensus(公议值)Accepted / Assigned(可接受/赋值).Accuracy

5、 (准确度)Expressed as (表示为)the ratio between the assayed value and the “true value (% recovery) 分析值与真值间的比(%回收率)the difference between the assay and the accepted true value (% Error)分析与可接受真值间的差(%误差).Precision(精细度)Closeness of agreement between measurements(丈量间的一致程度)Repeatability (r) same conditions, sho

6、rt time interval (same run) short term precision反复性(r)-一样条件下短时间间隔-短期内精细度Intermediate precision same lab different day, analyst, instrument 中间精细度-同一实验室不同日期,分析人员,仪器Reproducibility (R) agreement between batches or between labs复现性-批间或实验室间的一致性.Precision (精细度)Expressed as Standard Deviation, Relative Stan

7、dard Deviation or Relative Percent Difference表示为规范偏向、相对规范偏向、相对百分差.Sensitivity灵敏度Degree of response to a change in analyte concentration resolution被分析物浓度变化的呼应变化程度-分辩率Lowest concentration that can be distinguished from background noise detection limit能从背景噪音识别出的最低浓度-检测限.Sensitivity 灵敏度Limit of detectio

8、n vs. Limit of quantification检测限与定量限Limit of detection (LOD) is the level that we can say whether an analyte is present or not检测限是我们判别被分析物能否存在的含量程度Limit of quantitation (LOQ) is the level that we can quantify the analyte with a specified accuracy (20%)定量限是我们按规定准确度20%能对被分析物量化的含量程度.Selectivity选择性Abili

9、ty to detect the analyte in a complex matrix检测复杂基体中被析物的才干Ability to exclude non-analyte species from signal经过信号排除非被分析物的才干Usually inversely related to sensitivity通常与灵敏度成反比.Linearity线性Ability to produce a response that is directly proportional to the concentration of the analyte所产生的反响与被分析物浓度成正比的才干Only

10、 holds true within a given range只在给定范围内是真实的.Linearity 线性Expressed as correlation coefficient (r) or coefficient of determination (r2)表示为相关系数(r)或测定系数(r2)r2=ssxy2/ssxx ssyy.Range范围The interval between the highest and lowest concentration for which the method has shown to have suitable levels of accura

11、cy, precision and linearity.在方法具有适宜的准确度、精细度和线性的条件下，最高和最低浓度范围.Robustness稳健性Ability of method to be unaffected by small changes in method (internal) conditions方法不因条件的较小变化内部而受影响的才干Temperature温度pHComposition of mobile phase流动相组成 Useful when method moves from development to production从方法开发到运用很有用.Ruggedne

12、ss稳度Ability of method to be unaffected by external conditions方法不受外界条件影响的才干Different analysts不同的分析人员Different laboratories不同的实验室Different reagent lots不同批的试剂Different instruments不同的仪器.Ruggedness 稳度Useful for technology transfer对技术推行很有用.Quality Control Measures质量控制手段Calibration standards校准规范Blanks空白Rec

13、overy studies回收率研讨Precision studies精细度研讨Sensitivity studies灵敏度研讨Detection Limit检测限Quantitation limit定量限. Calibration (校准)Directly affects accuracy(直接影响准确度)Preparation of standards(规范制备)Matrix (基体)Stability(稳定性)Signal type: peak area, peak height信号类型:峰面积,峰高.Calibration (校准)Calibration curves(校准曲线)1st

14、 order straight line(一级-直线)Quadratic acceptable but requires more points(二次方程-可以接受,但需求更多点)Internal standards(内标)Refines calibration response(加强校准呼应)Added to samples and standards(参与样品和规范中)Must behave like the analyte(象被分析物一样表现)Cannot be in samples rare elements, deuterated compounds(样品中没有-稀有元素,含重氘的化

15、合物).Calibration (校准)Calibration verification (校准验证)Repeated calibration standard反复校准规范Interval may be every 20 samples (ICPMS) or once every run (GC-FID)间隔:20个样品(ICPMS) 每次(GC-FID).Blanks(空白)Used to monitor contamination(监测污染)Reagent blanks(试剂空白)Instrument blanks(仪器空白)Field blanks(场地空白)Trip blanks(路途

16、空白)Procedural / method blanks(程序/方法空白)Matrix blanks(基体空白)Others?(其它).Recovery Studies回收率研讨Used to monitor accuracy监测准确度Matrix spikes基体加标Fortified blanks添加加标Surrogates替代Reference Materials参考物质.Matrix Spikes基体加标Known amount of analyte added to sample在样品中参与知量的被分析物Important with complex matrix对复杂基体很重要Ge

17、nerally added prior to extraction process通常在提取前参与Sometimes difficult to know amount to spike ahead of time有时很难提早知道加标量.Fortified Blanks加强空白Analyte spike into reagent blank在试剂空白中参与被分析物标样Carried through sample preparation process在样品预备过程中参与.Surrogate替代Compound with similar properties to target analyte与被

18、分析物具有相近特性的化合物Added to all samples (unknowns and QC) but not standards在一切样品(未知的和QC)中参与，但标样中不加Used to monitor method performance on a sample (matrix) specific basis 应基于特定样品基体，用于监测方法表现. Reference Materials参考物质Matrix matched materials with known concentration of analytes被分析物知浓度的基体匹配的物质May be external or

19、 in-house外部 或室内Sources来源NIST (US)NRC (Canada)European Union欧盟Commercial Vendors商业渠道.Reference Materials参考物质Used primarily to monitor accuracy主要用于监测准确度May be used for other quality 用于其它质量目的measures (precision, sensitivity)丈量精细度、灵敏度Best overall QC?最好的全面质量控制？Expensive费用高.Precision Studies精细度研讨Duplicate

20、s反复Field duplicates场地反复Lab duplicates实验室反复Instrument duplicates仪器反复Inter-lab splits室内分样Used to identify variance in different processes用于识别不同过程的变异.Sensitivity Studies灵敏度研讨Usually performed initially, then periodically thereafter通常最开场要做，以后定期做Multiple replicates of a blank or low-level standard空白或低含量规

21、范多次反复.Sensitivity Studies灵敏度研讨Detection Limit no quantitation检测限-非定量Quantitation Limit Accuracy criteria added定量限准确度准那么.Sensitivity Studies灵敏度研讨Detection Limit 99% certainty that the concentration is greater than zero that the analyte is present in the sample检测限99%确定浓度大于0-样品中有被分析物Uncertainty is high

22、 (+/- 100% or more)不确定度高 +/- 100% 或更高Quantitation Limit定量限Lowest concentration that can be determined with a given accuracy (e.g. 20% relative error)在一定准确度下如20%相对误差可以测定出的最低浓度.Linearity线性Determined initially and then as needed最开场时测定，然后需求时测定Dynamic Linear Range relates to detector response动态线性范围与检测器呼应

23、有关Also consider preparation limitations也可以以为是预备中的限制Solubilities溶解度Extraction efficiencies提取率Derivitizing reactions衍生反响.What do we run as QC?为什么要做质量控制It depends on:取决于Type of instrumentation仪器类型Stage of Method Development方法开发阶段Type of analysis分析类型.What do we run as QC?为什么要做质量控制Stage of Method Develop

24、ment方法开发阶段Validation确认Verification / Qualification验证/判别Routine analysis日常分析.What do we run as QC?为什么要做质量控制Type of Analysis分析类型Assay分析Impurities杂质Limits限制Content含量Identification识别.Quality Data Required at Method Validation方法确认所需的质量数据DataRequired所需数据I.D.名称Impurity Testing杂质检测Assay Content分析含量Quant.量Li

25、mit限Accuracy准确度NOYESNOYESPrecision精密度NOYESNOYESSelectivity选择性YESYESYESYESDetection limit检测限NOMAYBE可能YESNOQuantitation limit定量限NOYESNOMAYBE可能Linearity线性NOYESNOYESRange范围NOYESNOYES.Quality Data Required in Routine Analysis日常分析所需质量数据DataRequired所需数据I.D.名称Impurity Testing杂质检测Assay Content分析含量Quant.量Limi

26、t限Accuracy准确度NOYESNOYESPrecision精密度NOYESNOYESSelectivity选择性NOMAYBE1NOMAYBE1Detection limit检测限NONONONOQuantitation limit定量限NOMAYBENOMAYBELinearity线性NOYESNOYESRange范围NONONONO1 may be required when working in unknown matrix.Review of Quality Assurance质量保证概述We will cover内容Definition and Description of Q

27、A质量保证的定义和描画Tools in a QA SystemQA体系的工具Proficiency Testing才干验证Certified Reference Materials有证规范物质Validated Methods经过确认的方法. Quality Assurance质量保证Quality Assurance质量保证Planned actions designed to provide confidence that quality requirements will be fulfilled为质量要求得到满足提供自信心而设计的有方案的活动Quality Assurance Syst

28、em质量保证体系A set of processes applied within a defined structure to generate desired outcomes在规定的构造内产生预期结果所采用的一组过程The good management of good science良好的科学良好的管理.Quality System Components质量体系组成Management管理Plan谋划Performance实施Do做Assessment评价Review评审.6 Pillars of QA/QCQA/QC的六个根底Management管理Facilities设备Perso

29、nnel人员CRMs有证规范物质PTs才干验证Validated Methods经确认的方法.Proficiency Testing才干验证Provides external assessment of performance为表现提供外部评审Provides a basis for corrective and preventive action为纠正和预防措施提供根底.Information Gained搜集信息Comparison of performance against an external standard将表现与外部规范比较Comparison against past pe

30、rformance与过去的表现比较Comparison against peer (competitor) labs与同行竞争者比较Identification of unsatisfactory performers识别出不称心的操作者.Types of PT才干验证类型Specific analyte/matrix combination特定被分析物/基体结合Mercury in fish鱼中的汞Benzene in air空气中的苯Field of analysis场地分析Metals by ICPICP测金属Pesticides by GC/MS GC/MS测杀虫剂.Samples样品

31、Sub-sampled from bulk supply从批中抽取样本Discrete sample split and distributed谨慎分割样品并分发.Interlaboratory Comparisons实验室间比对Collaborative studies协同研讨Certification studies认证研讨Round-robin studies循环研讨.Selection of PT programsPT方案的选择Availability of relevant programs能否有相关方案Organization of relevant programs相关方案的组织

32、Any program is usually better than nothing只需求方案，总比没有好.Assessment of PT ProgramsPT方案的评价Before committing long-term consider在实施前应思索Statistics used to interpret data解释结果的统计技术How “true value is determined真值如何确定Theoretical实际值Referee lab参考实验室Consensus公议值.Scoring of Participants参与者的评价Z scoreZ值Deviation fro

33、m “true value divided by sigma测得值与真值之差除以Sigma may be an accepted deviation or statistically determined in each round能够是可接受的偏向或每轮测试的统计结果.ScoringZ-值Generally a Z-score Z-值 2, 3 is considered unsatisfactory离群 scores must be within 2 sigmaZ-值必需在2- 之间.Laboratory Interpretation实验室的解释View results in contex

34、t从整体上看结果Do they agree with in-house QC data能否与室内质量控制数据一致Trend analysis (consider how sigma is determined)趋势分析思索是如何确定的Performance of other participants其它参与者的表现.Laboratory Interpretation实验室的解释Compare methodology and re-calculate if possible比较方法，假设能够重新计算Compare uncertainty against in-house estimates将不确

35、定度与室内评价比较.Corrective Actions纠正措施Determine when to take action确定何时采取措施After 1 unsatisfactory score?一个不称心结果After many (3) in one round?一轮中多个如三个不称心结果After 2 consecutive unsatisfactory scores?延续二个不称心结果.Corrective Actions纠正措施Always investigate总要调查Include包括QC data质量控制数据Calculations, dilutions, transcripti

36、ons计算、稀释，誊写Training status of analyst分析人员培训情况Performance records of equipment设备运转记录Records of calibrants, reagents etc.校准品、试剂的记录等.Corrective Actions纠正措施Formulate action公布措施Execute action实施措施Check if action was successful检查措施能否有效.General Considerations几点思索More emphasis is being placed on PT programs

37、by assessors, regulators and clients评审员、管理部门和客户更多强调PTUse all the information available利用一切可得到的信息Handle PTs like routine samples (as much as possible)象常规样品一样处置PT样品尽能够.Third Party Assessment第三方评审Accreditation Bodies认可机构Assess performance against laboratory scope rather than PT program criteria在一定范围内评审

38、实验室的表现，而不是PT方案准那么Consider “fit for purpose思索适宜性.Third Party Assessment第三方评审Regulators政府管理部门May be involved in development of PT programs能够参与PT方案的开发May require assistance from program coordinator to assess results能够需求方案协调人来协助评审结果.Third Party Assessment第三方评审Customers客户When using PT results as a perfor

39、mance standard ensure target is realistic当运用PT结果作为才干规范时，确保目的是现实的Must investigate program; not just results必需调查方案，而不仅是结果.Reference Materials参考物质5 types5种类型Pure substance纯物质Standard solutions and gas mixtures规范溶液和气体混合物Matrix RMs基体参考物质Physical properties物理特性Reference objects (artifacts)参考目的参考品.Referenc

40、e Materials参考物质May be used for 可用于Internal QC内部质量控制Method validation方法确认Calibration校准Estimating uncertainty评价不确定度Training培训.Classification分类Certified Reference Materials有证参考物质Directly traceable直接溯源Each property has an uncertainty associated with it每一特性有相应不确定度Reference material参考物质Properties are homogenous and thoroughly characterized to be used for calibration or method assessment特性是均匀的，并完好定值，以用于校准或方法评价.Avai