GLP(良好实验室规范).ppt

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1、GLP(良好实验室规范),国家为了保证药品的质量安全制定的一系列规范，包括：GAP中药材生产质量管理规范 GMP药品生产质量管理规范 GLP药物非临床研究质量管理规范 GCP药物临床试验管理规范（Good Clinical Practice）GSP药品经营质量管理规范GUP药品使用质量管理规范这些严格的规范被逐渐应用到其它相关领域，尤其是食品行业：GAP（Good Agricultural Practice）:良好农业规范GMP（Good Manufacturing Practices）:良好操作规范GLP（Good Laboratory Practice）:良好实验室规范GSP（Good S

2、upplying Practice）：良好经营（供应）规范,GLP(良好实验室规范),GLP是英文Good Laboratory Practice 的缩写，中文直译为良好实验室规范。GLP是就实验室实验研究从计划、实验、监督、记录到实验报告等一系列管理而制定的法规性文件，涉及到实验室工作的所有方面。它主要是针对医药、农药、食品、食品添加剂、化妆品、兽药等进行的安全性评价实验而制定的规范。制定GLP的主要目的是严格控制化学品安全性评价试验的各个环节，即严格控制可能影响实验结果准确性的各种主客观因素，降低试验误差，确保实验结果的真实性。,GLP(良好实验室规范),GLP始于20世纪70年代。新西兰

3、是第一个建立实验室登记法的国家。1976年美国食品药品管理局（FDA）制定了仅限于药品的GLP规范草案。1980年由美国联邦环保局（EPA）在联邦杀虫、杀菌、杀鼠剂法中发布了有关农药的GLP标准。加拿大、日本、韩国等国家先后发布了本国的GLP法规。欧共体在1975年5月公布了关于药品药理毒理、临床及临床标准草案法规，在1986年提出GLP草案，1988年又发布GLP检查法令。欧共体GLP与经济合作与发展组织（OECD）的GLP原则一致。1993年12月我国原国家药品监督管理局颁布了“药品非临床研究质量管理规定”(试行)。国家环境保护总局等部委也先后制定了本行业的GLP标准。我国农药行业GLP工

4、作始于2002年。,GLP(良好实验室规范),CONTENTS 内容,1、整洁有序的实验室日常管理 GOOD HOUSEKEEPING PRACTICE2、安全规范 SAFETY PRACTICE3、符合专业要求的操作 GOOD OPERATIONAL PRACTICE4、纯净水 PURIFIED WATER5、标准物质 REFERENCE MATERIALS6、标准溶液 STANDARD SOLUTIONS7、留样 RETAINED SAMPLES8、实验室器皿的清洁 CLEANING OF LABORATORY WARE9、化学通风橱 FUME CUPBOARDS10、层流通风柜（超净工作

5、台）LAMINAR FLOW HOODS11、实验室能力验证 LABORATORY PROFICIENCY TEST,现场的5S！,GLP(良好实验室规范),1、GOOD HOUSEKEEIPNG PRACTICE整洁有序的实验室日常管理,Work flow:A well organized laboratory should minimize the amount of backtracking and retracing of steps.工作流程：实验室的布置应合理有序，以有助于提高工作效率。Labs shall be kept clean and tidy and free from

6、unnecessary clutter and equipment.实验室应保持清洁，整齐，不放置不需要的物品和仪器。All gangways,aisles and exits will be free to allow easy access.通道，走廊和出口保持通畅。All equipment,glassware and other supporting instrumentation will be back in their proper place after use.所有仪器，玻璃器皿和辅助器具使用后应放加原处。A label will be placed on each cupb

7、oard and draw to identify its contents.橱柜和抽屉应有标识。Most chemicals in the laboratory are potentially hazardous,they shall be properly labeled and separately stored.化学品应分类存放，并按性质作危害性标识。,现场的EHS！,GLP(良好实验室规范),2、SAFETY PRACTICE-1 安全规范,Personnel will wear durable clothing that covers the arms,legs,torso and

8、 feet.Open-tode shoes and sandals will not be worn.实验室人员应穿着牢固的能遮盖手臂、腿、身体和脚的服装，不得穿着露趾鞋和拖鞋。A clean,fastened cotton laboratory coat will be worn.Laboratory coats will not be worn in refreshment areas or lunch rooms.应穿着紧身的棉质工作服，工作服不可穿进茶点休息区域或食堂。Eye protection will be worn unless the analyst can demonstr

9、ate that adequate protection is provided by other means.实验室应配备保护眼睛的设施，否则应配戴护眼镜。Each laboratory has dedicated hand washing facilities-including soap and paper towels.Hands are washed on entering the laboratory before starting analysis,and when entering and exiting the laboratory for lunch or going to

10、 the toilet.实验室应配备专用洗手设施-包括清洁剂和纸巾。进入实验室开始分析前，离开实验室进餐厅和由餐厅回实验室，或去洗手间均须洗手。,现场的EHS！,GLP(良好实验室规范),2、SAFETY PRACTICE-2 安全规范,Appropriate gloves are worn when handling substances that may be absorbed through the skin or that are corrosive,harmful or may irritate the analyst.处理易被皮肤吸收或腐蚀有害或刺激性的物质时应带适当的手套。Cha

11、racters of chemicals,such as“Flammable”,“Corrosive”etc.shall be correctly identified and labeled.化学品的特性，如“易燃”，“腐蚀”等应正确标识。Cylinders shall be fixed and clearly labeled.钢瓶应清楚标识，并固定。Cuts and grazes to the skin are adequately covered by suitable dressings.伤口和皮肤擦破处应适当地包扎敷裹。Personnel will not work in a lab

12、oratory alone.不可单独在实验室工作。Eating,drinking and smoking are prohibited in the laboratory at all times.任何时候均不得在实验室吃、喝和抽烟。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-1符合专业要求的操作-试剂的使用与配制-1,Solvent bottles are always covered as they will readily absorb moisture and contaminants from the air.溶剂易吸收空气中的水分和污染物，溶

13、剂瓶必须随时盖紧。A pipette will not be used to pipette directly from the bottle unless it is an automatic pipette.The remaining solvent is not returned to the stock bottle.It must be treated as waste.不可用移液管直接从瓶中移取溶剂或溶液，应倾倒入容器内移取，剩余溶剂不可倒回贮液瓶，应作废弃物处理。A spatula or spoon will not be placed directly into the bot

14、tle for solids.The required quantity is decanted into another container from which the material will be retrieved.The remaining material will not be returned to stock bottle.It should be treated as waste.不可用刮勺或匙直接从瓶中取用固体试剂，应在另一容器中倾入所需量。剩余试剂不可倒回原容器，应作废弃物处理。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-2符

15、合专业要求的操作-试剂的使用与配制-2,Laboratory personnel shall be made aware of their responsibilities in the use of suitable reagents,solvents,culture media,reference materials and laboratory ware in terms of the types of analysis they conduct.实验室人员应明确其有责任根据所进行的测试使用适合的试剂、溶剂、培养基、参照物和实验室器皿。Any possible contamination

16、,including Leftovers that has been returned to the containers.任何可能导致污染的操作，包括将取出未用完的试剂、溶剂、培养基、参照物放回容器，受影响的物质均应视为失效。INTEGRITY OF REAGENTSAll reagent containers shall be labeled and tightly closed.They shall bear the original label.所有试剂容器均应标识和盖紧。容器上的标贴必须为原标贴。INTEGRITY OF REAGENTS,GLP(良好实验室规范),3、GOOD OP

17、ERATIONAL PRACTICE-3符合专业要求的操作-试剂的使用与配制-3,The person responsible for the preparation of the reagent shall be identifiable either from the label or from records.试剂的配制人应在标贴上标识或在记录中写明。Laboratory shall establish written procedures for preparation of reagent solutions and culture media.Records of such pre

18、paration shall be maintained.实验室应建立试剂溶液和培养基配制方法的文件。应保存配制记录。Records for reagent solutions shall include measured weights and volume,burette readings,pH readings,calculation of standardization factor and solution concentration.试剂溶液配制记录应包括重量，体积，滴定管读数，PH读数标定因子的计算和溶液浓度。,GLP(良好实验室规范),3、GOOD OPERATIONAL PR

19、ACTICE-4符合专业要求的操作-试剂的使用与配制-4,The preparation record for culture media shall include medium name,batch number,amount prepared,pH before and after autoclaving autoclave time and pressure.培养基的配制记录应包括名称、批号、配制量、压热锅处理前后的PH值，处理时间和压力。Where laboratory prepares its own media,the chemicals used for such prepar

20、ation shall be verified to be of the appropriate quality before use.如实验室自己制备培养基，使用前应确认所用化学品符合质量要求。“hazardous substance”shall be kept separately from other reagents and held in locked cabinets.危险物质应与其它试剂分别存放，并加锁。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-5符合专业要求的操作-试剂的使用与配制-5,Preparation And Storage O

21、f Culture media培养基的制备和存储Culture media must be prepared and stored at the specified temperature and under the specified conditions according to the manufacturers instructions or method requirements.Each lot of prepared or purchased culture media must verified for its effectiveness.培养基必须按照制造商的说明或方法要求在

22、规定的温度和条件下制备和存放。无论是购买的或制备的培养基，其有效性必须验证。Prepared Plates of Culture Media:Poured plates of agar Media are especially vulnerable to infection,dehydration and chemical degradation.Aseptic preparation and storage are essential to protect plates from microbial infection.培养基制备平板，例如琼脂倾注平板，特别易受微生物侵染，脱水，和化学降解，

23、为使平板不受微生物侵染，必须进行无菌制备和存放。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-6符合专业要求的操作-试剂的使用与配制-6,GR(Guaranteed reagents)保证试剂（优级纯）（一级）绿色AR(Analytical reagents)分析纯（二级）红色CP(Chemical pure)化学纯（三级）蓝色LR(Laboratory reagents)实验试剂（四级）中黄色Correctly Select Reagents 正确选用试剂GR:用于精密度和准确度较高的分析AR:用于常规分析工作CP:通常不用于分析工作，尤其不适合配制标准

24、溶液LP:不适合用于分析工作此外，有特定用途的试剂纯度有高纯试剂，如光谱纯、色谱纯等。AR can be used for preparing standard solutions but not for standardization.分析纯试剂可用于配制标准溶液，但不可用于标定。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-7符合专业要求的操作-称量过程-1,Glass vessels used to weigh material will not be wiped with a dry cloth as this causes static elec

25、tricity build up in the container.Do not put material to be weighed in the weighing dish more than 2/3 of its volume.用于称量样品或试剂的玻璃器皿不可用干织物擦试以免产生静电。样品不能超过称量皿体积的2/3。All samples and containers are at the same temperature as the weighing device.Therefore,all materials are allowed to equilibrate to room t

26、emperature prior to use.所有样品和容器应与称量装置置于同一温度，以使所有物料使用前在室温下平衡。All weighing devices are calibrated or verified prior to use.Verification shall be conducted at and 2 times of target value.称量仪器使用前应校验或验证，验证应在1/2及2 倍目标称量值处进行。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-8符合专业要求的操作-称量过程-2,Bare hand can never to

27、uch the weights,clean gloves should be worn.不可用手接触砝码，应佩戴干净手套。Oven should be equilibrated at specified temperature prior to testing the loss of weight on drying.Sample after drying shall be cooled for a fixed and constant time interval.进行干燥失重测试前，应先将烘箱开启在规定温度下达到平衡。干燥后样品的冷却时间应恒定。Properly place objects

28、being dried in the desiccator,no stacking is allowed.在干燥器中的物体不可叠放。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-9符合专业要求的操作-容量器具的使用-1,The use of drying solvents(e.g.acetone),compressed air and paper towels will be avoided,where possible,as these may be other sources of damage or contamination.尽可能避免使用干燥溶剂

29、（如丙酮），压缩空气和纸巾以免可能的损坏或污染。Glass stoppers purchased with the volumetric flasks will remain with that flask.容量瓶的玻璃塞须保持原配。Use of pipettes:the solutions are not mouth pipetted irrespective of their nature.任何溶液均不可用移液管通过嘴吸取。All pipettes are inspected carefully prior to use.It will be checked for cracks in t

30、he tip;if present it will be discarded.Pipettes are clean and dry prior to use.移液管在使用前应检查顶端是否有裂纹；移液管使用前必须清洁干燥。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-10符合专业要求的操作-容量器具的使用-2,The pipette is rinsed at least twice with the sample solution before use.移液管使用前应至少用样品溶液润洗两次。When removing solution from a flas

31、k,sufficient volume is drawn to slightly above the mark,the solution is allowed to draw down to the mark by touching the tip of the pipette to the flask surface.Any excess fluid from the pipette is wiped in a downward motion then the aliquot is delivered.当由容量瓶移出溶液时，溶液体积应略高于刻度，然后用移液管尖端接触溶量瓶表面的方法将溶液调节

32、至刻度。Note:most pipettes are designed not to be expelled(i.e.liquid should remain in the tip after use).多数移液管都无须将残留液赶了（即将残留液留在移液管尖端）。Volumetric glassware can not be kept in heating environment,or in refrigerator or cooling cabinet.Do not hold the quantitative part of the volumetric glassware with hand

33、.所有容量器具不能存放在加热环境下或冰箱内。使用时不能用手捂住容量部分。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-11符合专业要求的操作-容量器具的使用-3,Graduated measuring cylinders are read by placing them on an even bench,and observing the meniscus at eye level.Volume is equivalent to the bottom of the meniscus.刻度量筒放置于平坦的桌面上读数，视线应与弯月面同一水平，由弯月面底部读取体

34、积。Items such as beakers,Erlenmeyer flasks and other glassware with rudimentary volume markings will not be used for measuring volume.带有粗刻度的器皿，如烧杯、三角瓶等玻璃器皿不可用于量度体积。All volumetric glassware shall be verified before use;Pipettes shall be verified once every 3 month,and auto pipettes verified daily befo

35、re use,record quarterly;Whether volumetric flask is verified quarterly shall be based on uncertainty contribution.All verification is recorded.所有容量器具使用前必须经过验证。移液管每三个月验证一次，移液枪每次使用前验证，并每三个月记录一次。容量瓶的验证根据它对方法结果的不确定度贡献在方法的SOP中注明是否需要每三个月验证一次。所有验证均须记录。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-12符合专业要求的操作-容

36、量器具的使用-4,All measurable glassware,such as pipette and volumetric flask,should be verified with certified thermometer,weights should also be certified and in calibration status.容量器皿（如移液管和容量瓶）的验证应使用处理校验状态的有证温度计及砝码.Volumetric measurement is an essential element in an analytical laboratory as many types

37、 of determination require specific dilutions and quantitative delivery of solutions.容量分析是分析实验室的基本内容，因为许多测试均涉及定量稀释和溶液的定量转移。Regardless of type of volumetric glassware,where accuracy is required,especially for quantitative analysis,all of such volumetric equipment shall be calibrated.容量仪器应恰当地维护和检查，任何容量

38、分析玻璃器皿,只要有精确度的要求，尤其是定量分析，所有这些仪器均应进行校验。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-13符合专业要求的操作-容量器具的使用-5,Coca-cola requires that“class A”glassware shall be used for volumetric analysis.Does this mean no calibration is necessary for any glassware marked“A”?可口可乐系统规定使用”A“级容量器皿，这是否意味着凡是标识”A“的容量器皿都不必要校验？甚至使

39、用了十余年也无需验证其是否仍符合A级要求吗？Is your Class A glassware supplied with a serialized certificate of precision?你的”A“级容量器皿有不重复编号的效证书吗？Glass A glassware need only be used where such volumetric accuracy is critical to the performance of the method and,where it is required,the glassware must be calibrated as confo

40、rming to Class A tolerance.A级玻璃器皿仅在容量准确性对方法结果而言为必须时才使用，当需要用A级时，必须校验以确认符合A级的容许误差。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-14符合专业要求的操作-容量器具的使用-6,Glassware used for measuring samples,standards and reagents for analytical procedures must be Class A.用于测量进行测试的样品、标准和试剂的玻璃器皿必须是A级。All plastic volumetric con

41、tainers are Class B.所有塑料容量分析容器均是B级。Syringes and automatic tip pipettors are not listed as Class A.注射器和自动移液管不列为A级。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-15符合专业要求的操作-样品处理,Sample preparation:All preparations will be done to mininize the potential risk of contamination or degrading the material to be

42、 analyzed.样品制备应将待测物质潜在的污染和降解或变质可能性降至最小。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-16符合专业要求的操作-记录保存,Recording Professionally.记录保存应符合规范。Log book is usually not original record.Adequate information and raw data,such as calculation,shall be maintained.数据表通常并非原始记录，记录应包含充分的信息及原始数据，例如计算。Record shall be made

43、 at the time when the activity is carried out,never do it afterwards.确保记录的实时性。避免任何形式的”补记“。,GLP(良好实验室规范),3、GOOD OPERATIONAL PRACTICE-17符合专业要求的操作-培训,A number of extraneous conditions may influence the precision of a given measurement.They include temperature,method of delivery,depth of color of the so

44、lution,type of meniscus,calibration to contain or deliver a definite volume,and so forth.Thus proper training of personnel and continuing observation of their operations shall be instituted as part of the quality assurance process to minimize or eliminate problems associated with these extrinsic fac

45、tors which can affect precise liquid measurements.许多外部条件将影响测试的精确性，例如温度，样品或溶液的转移方法，溶液颜色深度，液柱弯月面的形状，确定体积的容量或转移量的校验等。因此，恰当的人员培训，操作的持续监视应成为实验室品质保证过程的一部分，以减少或消除这些影响液体精确测量的外部因素。,GLP(良好实验室规范),4、PURIFIED WATER-1 纯净水,Purified water is one of the most critical but most often neglected reagents used in laborat

46、ory operations.Use of improperly purified water may account for the failure of analysis.水是最重要而常被忽视的试剂之一，使用不合格的水可能会导致分析的失败。Distillation of water will not always ensure quality.The materials and construction of the distiller,and the character of raw water all influence the quality of the distillate.Th

47、e storage container,too,can significantly influence the purity of the water.蒸馏并不总能确保水的质量，蒸馏装置的材质和构造，以及原水的品质均影响蒸馏水的质量。储存容器也将显著地影响蒸馏水的质量。,GLP(良好实验室规范),4、PURIFIED WATER-2 纯净水,Stills need periodic cleaning to remove scale.蒸馏装置需定期清洁和除垢。For more precise analysis,it may be necessary to use water distilled

48、from quartz or all-borosilicate glass distillation system.要求较严格的分析可能需使用石英硼硅玻璃蒸馏装置精馏的水。Purified water can be defined as water that has been distilled and/or deionized so that it meets relevant standard or specifications.纯净水为经蒸馏和/或去离子的水，以达到或高于相关的标准或规格。,GLP(良好实验室规范),4、PURIFIED WATER-3 纯净水,分析实验室用水国家标准一、

49、二、三级实验室用水的技术指标（GB6682-92),一级水用于有严格要求的分析实验，如液相色谱分析用水等。二级水用于无机痕量分析，如原子吸收光谱分析用水等。三级水用于一般的分析工作。,GLP(良好实验室规范),4、PURIFIED WATER-4 纯净水,Grade 1 water should be produced by further treatment of grade 2 water,for example by reverse osmosis or ion exchange followed by filtration through a membrane filter of po

50、re size 0.2m to remove particle matter or re-distillation from a fused silica apparatus.一级水可用二级水经过石英设备蒸馏，或离子交换或反相渗透再经0.2m孔径的薄膜过滤器处理获得。Grade 2 water can be produced by multiple distillation.Re-distillation can also use sub-boiling silica distillation apparatus.二级水可用多次蒸馏或离子交换等制得，二次蒸馏水一般可达到二级标准。第二次蒸馏也可