仪器确认 附件2 GC确认 中英文doc.docx

1、仪器确认 附件2 GC确认 中英文docOMCL Network of the Council of EuropeQUALITY ASSURANCE DOCUMENT质量保证文件PA/PH/OMCL (06) 86 DEFQUALIFICATION OF EQUIPMENT仪器确认ANNEX 2: QUALIFICATION OF GC EQUIPMENT附件2：气相色谱仪的确认Full document title and reference 文件全名和索引号Qualification of EquipmentAnnex 2: Qualification of GC EquipmentPA/

2、PH/OMCL(06)86DEFDocument type 文件类型GuidelineLegislative basis 立法基础The present document was also accepted by EA as recommendation document to be used in the context of Quality Management System audits of OMCLsDate of first adoption 首次发行日期May 2006Date of original entry into force 首次执行日期June 2007Date of

3、 entry into force of revised document 修订后执行日期October 2006Previous titles/other references 原文件名/其它索引号This document replaces part of document PA/PH/OMCL(06)46 DEFCustodian Organisation 保管机构The present document was elaborated by the OMCL Network/EDQM of the Council of EuropeConcerned Network 相关网络GEONAN

4、NEX 2 OF THE OMCL NETWORK GUIDELINE“QUALIFICATION OF EQUIPMENT”OMCL网络指南“仪器确认”附件2QUALIFICATION OF GC EQUIPMENT气相色谱仪的确认Introduction 介绍The present document is the second Annex of the core document “Qualification of Equipment”, and it should be used in combination with it when planning, performing and d

5、ocumenting the GC equipment qualification process.本文件是核心文件“仪器确认”的第二个附件，在计划、实施和记录气相色谱仪的确认时，应将本文件与核心文件联合使用。The core document contains the general introduction and the Level I and II of qualification, common to all type of instruments, and the present annex contains GC instrument-related recommendation

6、s on parameters to be checked and the corresponding typical acceptance limits, as well as practical examples on the methodology that can be used to carry out these checks.核心文件包括了一般介绍和第一级与第二级确认，适用于所有类型的仪器，本附件包括了气相色谱仪相关的建议，包括哪些参数需要检查，相应的典型可接受标准，以及用来进行这些检查的实践方法学例子。The tests proposed in the Level III an

7、d IV of qualification are based on an overall approach, in which several parameters are checked at the same time in a combined test procedure, to obtain information on the overall system performance (e.g. peak area precision, retention time precision, temperature programme reproducibility, etc).在第三级

8、和第四级确认所建议的检查是基于一种全面检查的方法，在其中同一个联合测试可以检查几个不同参数，得到全面的系统性能信息（例如峰面积精密度、保留时间精密度、温度程序重复性等）Nevertheless, it should be noted that it is also acceptable to check these parameters individually by using other well-defined procedures.另外，需要注意如果采用其它界定很好的程序对这些参数进行单独确认也是可以接受的。TABLE III表3Level III. Periodic and moti

9、vated instrument checks第三级 周期主动仪器检查Examples of requirements for GC instruments with FID配备FID检测器的气相色谱仪的要求举例Instrument module仪器模块Parameter to be checked需要检查的参数Typical tolerance limit典型可接受限度1 Inlet system进样系统1.1 Injector leak test 进样器泄漏检查1.2 Pressure/flow accuracy and stability 压力/流速准确性和稳定性1.3 Repeatab

10、ility of injection (overall test 1)- in split mode 分流模式-In split less mode 分流较少模式1.4 Injector temperature ands accuracy and stability 进样器温度 准确度和稳定性1.5 Carry-over (overall test 3) 残留（全面检查3）Pressure drop15kPaWithin 5 min5分钟内压降15kPaCovered by overall test 1包括在全面检查1中RSD3.0%RSD3.0% Covered by overall tes

11、t 2包括在全面检查2中0.2% 2. Oven柱温箱2.1 Repeatability of oven temperature characteristics 柱温箱温度重复性Covered by overall test 2包括在全面检查2中3. FID detectorFID检测器3.1. Linearity (overall test 3)线性（全面检查3）3.2. Constant detector response 检测器响应恒定性3.3 Noise噪声3.3. Drift 漂移r20.999covered by overall test 1 or 2包括在全面检查1或2中see

12、annex 1 见附件1See Annex 1 见附件2TABLE IV 表四Level IV. In-use instrument checks 第四级：在用仪器检查Examples of requirements for GC instruments with FID 配置FID检测器的气相色谱仪为例Parameter to be checked 需要检查的参数Typical tolerance limits典型可接受限度1.System suitability check for the method方法系统稳定性检查According to Ph. Eur. Or MAH dossie

13、r or validated in-house method根据EP或MAH相关文件，或内部已验证的方法2.Peak area precision峰面积精密度RSD3.0% unless otherwise prescribed*除另有规定外RSD3.0%3.Retention time repeatability保留时间重复性RSD2.0%4.Sensitivity (where relevant, e.g. for related substances tests)灵敏度（如果相关，例如对于有关物质）According to Ph. Eur. or MAH dossier or valid

14、ated in-house method根据EP或MAH相关文件，或内部已验证的方法* This is to be defined in conjunction with the target concentration of the analyte这要与分析物的目的浓度联系起来确定。All parameters given here should be checked when performing analyses under the working conditions for the actual sample determinations. Normally, the test an

15、d reference solutions to be prepared for this purpose are given as a part of the method.这里给出的所有参数应在工作状态下进行实际样品检查分析时进行检查。一般来说，供试液和对照溶液应根据此目的作为方法的一部分进行准备。ANNEX I 附件1Level III. Periodic and motivated instrument checks第三级 仪器周期主动检查Practical examples of tests and their associated tolerance limits for seve

16、ral parameters related to the performance of the different modules of a GC are presented below.下面是与不同GC模块的性能相关的几个参数检查的实践例子和其相关的允许限度These examples can be considered by the OMCLs as possible approaches to perform the Level III of the equipment qualification process: “Periodic and motivated instrument

17、checks”.这些例子可以认为是OMCL可以使用的进行第三级仪器确认“周期主动的仪器检查”的方法Several tests are proposed to check various parameters at the same time (overall tests). In order to run the tests in a more economical way, other suitable solutions can be used, as for example, the “Grob Test” mixture, available from different suppli

18、ers (e.g. Alltech, Sigma, Thames Restek). This commercial solution should be appropriate to the column material used.建议同时检查几个参数（全面检查）。为了采用更经济的检查式，也可以使用其它合适的溶液，例如“Grob Test”混合物，可以从几个供应商处采购（例如Alltech, Sigma, Thames Restek）。这个商业化溶液应适用于色谱柱材料。It is recommended to run the overall test by using always the

19、same test column, exclusively dedicated to qualification purposes, to guarantee reproducible conditions.建议一直采用同一根色谱柱进行全面检查，该色谱柱专用于仪器确认，以保证条件的可重复性1. INLET SYSTEM 进样系统The following tests are proposed for the periodic and motivated check of the GC Inlet System.建议对GC进样系统周期主动检查实施以下内容1.1. INJECTOR LEAK TE

20、ST 进器器泄漏检查Method:方法If not otherwise specified by the instrument manufacturer, the leak test is carried out according to the procedure laid down in the instrument manual or by the built in automatic leak check procedure of the instrument.如果仪器供应商未另行指明，泄漏检查应根据操作手册指定的程序来进行，或者由仪器的内置泄漏自动检测程序进行。Otherwise u

21、se the test described below:否则采用以下所述检查Disconnect the column from the injector and close the injector outlet with a sealed cap.断开柱子与进样器连接，封闭进样器出口Close the septum purge and the bypass.关闭隔垫吹扫和旁路吹扫Adjust the flow and pressure controller to the maximal possible value of the pressure gauge.调整流速和压力控制器至可能的压

22、力最大值Adjust the flow controller to zero.调整流速并控制在0Read the pressure after 1 minute and record the value.在1分钟后读取压力值并记录Record the pressure after 5 minutes.在5分钟后记录压力值Limits:限度Pressure drop 15 kPa within 5 minutes.5分钟内压降 15 kPa1.2. INLET PRESSURE/FLOW ACCURACY AND STABILITY 进样压力/流速准确性和稳定性A direct measurem

23、ent of these parameters was not deemed practical or necessary, but the optimal conditions of flow/pressure can be verified by the overall test 1.直接对这些参数进行测量在实际中不可行或没有必要，但流速/压力的最好条件可以在全面检查1中进行确认。Limits: refer to overall test 1.限度：参见全面检查11.3. REPEATABILITY OF INJECTION 进样重复性The verification of this pa

24、rameter is covered by the overall test 1.本参数的确认可以包括在全面检查1中This test is to be performed in both split and split less mode.检查应针对分流和少分流两种模式Limits: refer to overall test 1.限度：参见全面检查11.4. INJECTOR TEMPERATURE ACCURACY AND STABILITY 进样器温度准确性和稳定性Due to the fact that the temperature cannot be reliably measu

25、red without opening and modifying the system and due to the difficulties of introducing a probe inside this module, the verification of this parameter is considered to be covered by the overall test 2.由于在不打开柱温箱和调整系统条件的情况下很难可靠地对温度进行测量，并且探头很难放入本模块中，因此本参数包括在全面检查2A和2B中。Limits: refer to overall test 2.限度

26、：参见全面检查21.5. INJECTOR CARRY OVER 进样器残留After having injected the solutions for the linearity test of the FID detector, in increasing order, inject the blank and measure the peaks that correspond to the major peaks (= analytes) in the linearity solutions.在FID检测器线性检查进样后，按浓度增加的顺序，进线性溶液空白并测量主峰（被分析物）。The

27、verification of this parameter is covered by the overall test 3.本参数的确认可以包括在全面检查3中Limits: refer to overall test 3.限度：参见全面检查32. OVEN 柱温箱2.1. REPEATABILITY OF THE OVEN TEMPERATURE CHARACTERISTICS 柱温箱温度的重复性Due to the fact that the temperature cannot be reliably measured without opening and modifying the

28、 system conditions and that even when introducing a probe inside the oven, its location would not reflect the real temperature conditions at all points, the verification of this parameter is covered by the overall tests 2A and 2B.由于在不打开柱温箱和调整系统条件的情况下很难可靠地对温度进行测量，即使将探头放入柱温箱中，其放置的位置也无法反映所有点的真实温度情况，因此本

29、参数包括在全面检查2A和2B中。Limits: refer to overall test 2.限度：参见全面检查23. FID DETECTOR FID检测器The following tests are proposed for the periodic and motivated check of the GC FID detector.下列检查目的是对GC的FID检测器进行周期主动性检查3.1. FID DETECTOR LINEARITY FID检测器线性Increasing amounts of analyte are injected and a linear response

30、should be obtained.注入一系列不断增加数量的被分析物，所得的响应值应呈线性。The verification of this parameter is covered by the overall test 3.本参数的确认包括在全面检查3中Limits: refer to overall test 3.限度：参见全面检查33.2. CONSTANT FID DETECTOR RESPONSE 恒定FID检查器响应The proper and reproducible functioning of the FID can be demonstrated by checking

31、 the peak areas obtained from a pre-defined standard solution.FID检测器的功能正确性及重复性可以通过检查预设定的标准溶液的峰面积得到。The verification of this parameter is covered by the overall test 1 or 2.本参数的确认可以包括在全面检查1或2中Limits: refer to overall test 1 or 2.限度：参见全面检查1或23.3. FID DETECTOR NOISE AND DRIFT FID检测器噪声和漂移If the instrument has a built-in automatic system for the verification of the noise and drift, follow the manufacturers instructions and apply the defined acceptance criteria. Otherwise, use the test described below:如果仪器有一个内置的自动系统进行噪声和飘移确认，应根据供应商的指示进行，并采用供应商的可接受标