仪器确认 附件3 紫外确认 中英文docWord文档下载推荐.docx

1、December 2007Previous titles/other references 原文件名/其它索引号This document replaces document PA/PH/OMCL （07） 11DEF Custodian Organisation 保管机构The present document was elaborated by the OMCL Network/ EDQM of the Council of Europe Concerned Network 相关网络GEON ANNEX 3 OF THE OMCL NETWORK GUIDELINE“QUALIFICATI

2、ON OF EQUIPMENT”OMCL网络指南“仪器确认”附件3QUALIFICATION OF UV-VISIBLE SPECTROPHOTOMETERSIntroductionThe present document is the third Annex of the core document “Qualification of Equipment”, and it should be used in combination with it when planning, performing and documenting the UV-Visible spectrophotomete

3、r qualification process.本文件是核心文件“仪器的确认”的第三个附件，在计划、实施和记录紫外-可见光分光光度计的确认时应与该核心文件结合使用。The core document contains the Introduction and general forms for Level I and II of qualification, which are common to all type of instruments.核心文件包括了对第一级和第二级确认的介绍和一般表格，它们适用于所有类型的仪器。For UV-Visible spectrometers, an exa

4、mple has been added to give instrument-specific proposals that may be used in combination with the general requirements presented in the core document “Qualification of Equipment”, when drawing up a Level I checklist.对于紫外-可见光分光光度计，增加了一个例表给出仪器相关的方案，可以在规划第一级检查清单时，与核心文件里的通用要求“仪器的确认”结合使用。The present ann

5、ex contains instrument-related recommendations on parameters to be checked at Level III and IV of qualification and the corresponding typical acceptance limits, as well as practical examples on the methodology that can be used to carry out these checks.本附件包括了仪器相关的推荐，其中有第三级和第四级需要检查的参数和对应的典型可接受限度，以及一些

6、可以实施这些检查项目的实践举例。TABLE I 表一Level I. Selection of instruments and suppliers 第一级 仪器和供应商选择Example of check-list （non-exhaustive） 检查清单举例（非完全清单）Manufacturer: 生产商Provider/Distributor: 供应商/分销商Name of instrument and type: 仪器名称和型号Attribute 特性（this list may be adapted if necessary）（必要时可以采用本清单）Specifications 标准

7、Benefits 益处（instrument/suppliers ）（仪器/供应商）Assessment评价Pass通过Fails不通过Spectrophotometer 光度计Single beam and double beam model 单光束和双光束模式Allow both modes允许双模式Wavelength range 波长范围190-900nmPhotometric range 光度计范围Minimum 2.0 absorbance （Abs.） unitLamp switching 灯开关Allow both modes manual or automatic 允许双模式

8、：手动和自动Band width 波段宽0.2-4.0nm or better with 0.1nm for increments0.2-4.0nm或更好，以0.1nm为步距变化Automatic baseline corrections自动基线校正Must 必须有Wavelength accuracy 波长准确性Minimum of 0.2nm最小Wavelength reproducibility波长重复性0.05nm or better0.05nm或更好Wavelength resolution波长分辨率0.2nm or better0.2nm或更好Photometric accurac

9、y光度计准确度0.003 Abs. units or better for 1.0Abs. unitsPhotometric stability 光度计稳定性After 2 hours should not be more than 0.0005Abs. units/hPhotometric reproducibility 光度计重复性Should not be more than 0.0005 Abs. units at 0.5 Abs. units在0.5Abs.单位时应不大于0.0005Abs。Photometric noise光度计噪音Should not be more than 0

10、.0003 Abs. units at 1.0 Abs. units在1.0Abs.单位时应不大于0.0003Abs.单位Scan speed 扫描速度 Should be between 0.25nm/sec. and 8nm/sec. or better应介于0.25nm/秒至8nm/秒之间或更好Monochromator slew rate单色器压摆率Should be 1500nm/min. or better 应为1500nm/分钟或更好Data acquisition and processing system 数据获得和处理系统Acquisition at more than o

11、ne wavelength 在不止一个波长获得数据Minimum of two最少2个Photometric scaling in Abs. units, %T, log Abs. units and concentration光度计刻度包括Abs.单位，T%，Abs.单位对数和浓度Abscise scaling in nm, min., deg, and mm.切除刻度包括纳米，分钟，度和毫米Calibration at one or more levels and one or more wavelengths在一个或多个水平，以及一个或多个波长进行校正Calculate and give

12、 factor for linear regression and other计算并给出线性回归因子和其它Build and memorise in file form: data, method and report创建并保存为文件形式：数据、方法和报告Accessories 附件Flow-through cuvette; holder for n cuvette（s）流动池，比色皿支架可以放置多少比色皿Thermostated cell holder （temperature range and stability）可控温比色皿支架（温度范围和稳定性）Filters for qualifi

13、cation checks确认检查用滤片Notes: 注 This check-list, containing examples of attributes that can be taken into account in the selection of an instrument and supplier, can be used in combination with the general check-list presented in Level I in the core document “Qualification of Equipment”. 本检查清单，包括了特性举例，

14、这些举例可以在仪器和供应商选择时参考，这份清单可以与核心文件“仪器的确认”中第一级通用检查清单结合使用。 For Table II （Level II of Equipment Qualification: Installation and release for use） please refer to the core document. 对于表二（第二级仪器确认：安装和使用放行），请参见核心文件TABLE IIILevel III. Periodic and motivated instrument checksExamples of requirements for UV-Visibl

15、e spectrophotometersParameters to be checked要检查的参数Typical tolerance limits典型允许限度1. Spectral slit width （if applicable）光狭缝宽度（如适用）10%2. Wavelength accuracy 波长准确度1nm for the UV range 紫外光范围内1nm3nm for the visible range可见光范围内3. Wavelength precision波长精密度 See manufacturers specifications见生产商规格4. Photometri

16、c accuracy （control of absorbance）光度计准确性（吸光度控制）See annex I见附件一5. Photometric linearity 光度计线性r20.9996. Limit of stray light杂散光限度A2.0 at 198nm7. Baseline noise基线噪声0.002 Absorbance units （500nm） or或0.01 Absorbance units （200, 300, 400nm）8. photometric drift光度计飘移0.001 Absorbance units/h （250 nm） Or或0.00

17、2 Absorbance units/h （500 nm）TABLE IV 表四Level IV. In-use instrument checks 第四级 仪器使用中检查Examples of requirements for UV-Visible spectrophotometers 紫外-可见分光光度计要求举例Parameter to be checked1. System suitability check of the method方法系统适用性检查 e.g. Repeatability 例如 重复性 e.g. Resolution （if required for qualitat

18、ive analysis） 例如 分辨率（如果定量分析需要的话）According to Ph. Eur. or MAH dossier or validated in-house method根据欧洲药典或MAH文件或经过验证的内控方法2. Absorption cells吸收池Absorbance difference 0.005吸光度差异0.005ANNEX I 附件1Level III. Periodic and motivated instrument checks 第三级 周期主动性仪器检查This Annex contains practical examples of test

19、s and their associated tolerance limits for several parameters related to the performance of a UV-Visible spectrophotometer.本附件包括与紫外-可见光分光光度计性能有关的几个参数的检查实例及其相关的允许限度These examples can be considered by the OMCLs as possible approaches to perform the Level III of the equipment qualification process: “P

20、eriodic and motivated instrument checks”.这些例子可以认为是OMCL在实施第三级仪器确认“周期主动性仪器检查”的可行性方法GENERAL CONSIDERATIONS 一般考虑 Measurements made by comparing samples against external standards should be made under conditions during which temperature is held constant. This is particularly relevant where the carrier so

21、lvent is organic and measurements may be distorted by expansion or evaporation of the solvent. 如果测量需要将样品与外标进行比较，则检测过程应保证温度恒度。尤其是如果载液是有机溶剂，测量结果可能会因为溶剂的膨胀或汽化而变化时。 It is recommended to perform the qualification within the spectral range corresponding to the region of analytical interest. 推荐根据分析范围所需进行光学

22、范围确认 Ensure that the spectrophotometer has stabilized, according to the manufacturers recommendations, before starting the qualification tests. 在进行确认检查前，应根据供应商的建议确保分光光度计稳定。 When references are made to the European Pharmacopoeia, e.g. reagents R, then the reagent quality complies with the EP specific

23、ations. 如果引用了欧洲药典，例如试剂纯度的试剂，那么试剂的质量符合EP质量标准。 When using commercial filters as alternative to the proposed tests, a set of filters covering the entire range of interest should be used. They should be calibrated with traceability to national/international standards, preferable through a national metro

24、logy laboratory or NIST. 如果使用商业化的滤液作为替代以进行检查，需要使用一套覆盖所需的整个范围的滤液。这些滤液应经过校正，可以追溯到国家的/国际的标准，最好是经过一个国家计量实验室或者NIST。1. SPECTRAL SLIT WIDTH （if applicable） 光学狭缝宽度（如适用）When using an instrument on which the slit-width is variable at the selected wavelength, the slit-width must be small compared with the half

25、-width of the absorption band but it must be as large as possible to obtain a high value of I0. Therefore, a slit-width is chosen such that further reduction does not result in a change in absorbance reading.如果使用的仪器在选择的波长处，其狭缝宽度可调节，则其宽度必须小于吸收波段的半宽，但必须足够大以得到较高的I0值。因此，需要对狭缝宽度进行选择使其进一步降低时不会导致吸光度读数变化。Me

26、thod and Limits:方法和限度1. Switch the system on and start the Scan module. 开机，启动扫描模块2. Select SETUP and set the following parameters:X Mode = NanometresX模式 = 纳米Start wavelength = 660.0 nm起始波长 = 660.0 nmStop wavelength = 650.0 nm结束波长 = 650.0 nmY Mode = % TY模式 = %TScan rate = 10 nm/min扫描速率 = 10 nm/minGai

27、n = （100） see 4 below增益 = （100）见下述第4项3. Select Options tab and set the following parameters:选择选项条，设定以下参数SWB = 4 nmBeam mode = Single front光束模式 = 单光束在前Lamps on = Deuterium开灯 = 氕Source change = 700.0 nm光源变化= 700.0 nm4. Start a scan and examine the trace for a spectral peak around 656.1 nm.开始扫描，在656.1n

28、m处检查光学峰的痕迹If no peak is seen or it is less than 50% T, increase the gain.如果看不到峰或少于50%T，提高增益If the signal exceeds 100% T, reduce the gain.如果信号超过100%T，降低增益5. Measure the width of the peak （in nanometres） at half the height of the peak.测量峰半峰高的宽度（单位nm）This represents the spectral bandwidth and should be within 10% of that selected via the computer.这代表光学带宽，且其应该在通过计算机选择的 10%之内。6. Check the calibrat