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1、OMCL Network of the Council of EuropeQUALITY MANAGEMENT DOCUMENTPA/PH/OMCL (11) 04QUALIFICATION OF EQUIPMENT仪器确认ANNEX 1: QUALIFICATION OF HPLC EQUIPMENT附件1：HPLC仪器的确认Full document title and reference文件全名和索引号Qualification of EquipmentAnnex 1: Qualification of HPLC equipmentPA/PH/OMCL (11) 04Document t
2、ype 文件类型Guideline 指南Legislative 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 2005Date of original entry into force首次执行日期June 2005Date of entry into force of revi
3、sed document 修订后执行日期1st July 2011Previous titles/other references原文件名/其它索引号This document replaces document PA/PH/OMCL (07) 17 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GEONANNEX 1 OF THE OMCL NETWORK GUIDEL
4、INE“QUALIFICATION OF EQUIPMENT”OMCL网络指南“仪器的确认”之附件1QUALIFICATION OF HPLC EQUIPMENTHPLC仪器的确认Introduction 概述The present document is the first Annex of the core document “Qualification of Equipment”, and it should be used in combination with it when planning, performing and documenting the HPLC equipmen
5、t qualification process.本文件是核心文件“仪器的确认”第1个附件，在计划、实施和记录HPLC仪器的确认过程时，应将本文件与核心文件一起使用。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 HPLC instrument-related recommendations on parameters to be
6、 checked and the corresponding typical acceptance Limits, as well as practical examples on the Methodology that can be used to carry out these checks.核心文件包括了第一级和第二级确认的通用介绍，适用于所有类型的仪器，本附件包括了HPLC仪器相关的需要检查的参数和相应典型的可接受标准的推荐，以及可用于进行这此检查的实用方法学举例。When qualifying HPLC equipment, it should be noted that it i
7、s acceptable to check at Level III and IV several of the mentioned parameters at the same time in a combined test procedure (e.g. “overall” system performance test giving information on peak area precision, retention time precision, gradient reproducibility, etc).在进行HPLC仪器确认时，应注意也可以对第三级和第四级几个提到的参数采用
8、联合检测程序同时进行检查（例如“全面”系统性能检查，同时给出峰面积精密度、保留时间精密度、梯度重复性等的信息）TABLE III 表三Level III. Periodic and motivated instrument checks第三级 定期主动仪器检查Examples of requirements for HPLC instruments and detectorsHPLC仪器和检测器要求举例Instrument module仪器模块Parameter to be checked需检查的参数Typical tolerance Limits典型允差限度Solvent delivery
9、system溶剂传送系统l Flow rate 流速l Proportioning accuracy and precision (gradient test) 配比准确度和精密度（梯度测试）l Proportioning ripple 配比波动l 5 %l 2l 0.2 %Injector进样器l Volume precision 进样量精密度l Carry-over 残留l RSD1.0 %l see Annex I 见附件1Autosampler自动进样器Thermostatting accuracy and precision 恒温准确度和精密度l 3 COven or cooling
10、 device柱温箱或冷却装置Thermostatting accuracy恒温准确度l 2 CUV/DAD detectorUV/DAD检测器l Linearity 线性l Wavelength accuracy波长准确度l r2 0.999l 2 nmFluorescence detector荧光检测器l Wavelength accuracy excitation波长激发准确度l Wavelength accuracy emission 波长发射准确度l Sensitivity 灵敏度l 3 nml 3 nml see Annex IElectrochemical detector 电化
11、学检测器l Accuracy of the signal 信号准确度l Stability of the signal 信号稳定性l see Annex I 见附件1l see Annex I 见附件1RID detectorRID检测器l Signal/Noise ratio 信噪比l Drift over time 飘移l see Annex I见附件1l 0.1 mV/minCD detectorCD检测器l Signal/Noise ratio 信噪比l Sensitivity 灵敏度l Drift over time 飘移l Linearity 线性l see Annex I见附件1
12、l see Annex I见附件1l see Annex I见附件1l r 0.999TABLE IV 表四Level IV. In-use instrument checks第四级 在用仪器检查Examples of requirements for HPLC instruments with UV or DAD detectors配备UV或DAD检测器的HPLC仪器的要求举例Parameter to be checked需检查参数Typical tolerance Limits限度l System suitability check for the Method方法系统适用性检查Accor
13、ding to Ph. Eur. or MAH dossier or validated in-house Method根据欧洲药典或MAH文件或公司内部经过验证的方法l Peak area precision (applicable to the main peaks in the test solution)峰面积准确度（适用于供试液中主峰面积）RSD 1.5 %(unless otherwise prescribed in the system suitability of the Method, e.g. specific requirements from Ph. Eur. 2.2.
14、46, API monographs or MA dossiers) 除非在方法的系统适用性里有描述，例如EP2.2.46特定要求，原料药各论或MA文件l Retention time precision保留时间精密度RSD 5 %l Carry-over (by comparing consecutive standard (of the substance being quantified) and blank injections) 残留（通过比较连续（进行定量检测的物质）标准和空白进样） 0.2 %l Signal/Noise ratio (to be applied for rela
15、ted substances test)信噪比（用于有关物质检测）According to Ph. Eur.根据欧洲药典ANNEX I 附件1Level III. Periodic and motivated instrument checks第三级 定期性的主动仪器检查This Annex contains practical examples of tests and their associated tolerance Limits for several parameters related to the performance of the different modules of a HPLC.本附件包括一些实用几个与HPLC不同模块相关的参数检测举例及其相应的可接受限度。These examples can be considered by the OMCLs as possible approaches to perform the Level III of the equi
