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近日，EDQM OMCL發(fā)布了《分析用色譜柱的確認(rèn)》指南，該文件概述了分析色譜柱確認(rèn)的一般原則。色譜柱被認(rèn)為是設(shè)備，作為色譜系統(tǒng)的重要組成部分，它們會(huì)影響分析結(jié)果。因此，OMCL 認(rèn)為必要時(shí)應(yīng)進(jìn)行色譜柱的確認(rèn)。

 

文件介紹了液相色譜（LC、HPLC、UHPLC）和氣相色譜（GC） 程序中使用的分析色譜柱的確認(rèn)要求和一般標(biāo)準(zhǔn)。

 

OMCL表示在計(jì)劃、執(zhí)行和記錄確認(rèn)過(guò)程時(shí)，在收到色譜柱時(shí)以及在色譜柱的生命周期中，都將其用作指導(dǎo)。

 

該文件現(xiàn)已翻譯完成，如下：

 

QUALIFICATION OF ANALYTICAL COLUMNS

 

分析用色譜柱的確認(rèn)

 

Note: Mandatory requirements in this guideline and its annexes are defined using the terms “shall” or “must”. The use of “should” indicates a recommendation. For these parts of the text other appropriately justified approaches are acceptable. The term “can” indicates a possibility or an example w ith non-binding character.

 

注：本指南及其附件中的強(qiáng)制性要求使用術(shù)語(yǔ)“應(yīng)”或“必須”進(jìn)行定義。使用“應(yīng)該”表示推薦。對(duì)于本文件中的要求，也可以接受其他適當(dāng)合理的方法。術(shù)語(yǔ) “可以” 表示具有非約束性特征的可能性或示例。

 

Contents 

 

目錄

 

1. INTRODUCTION

 

介紹

 

2. SCOPE

 

范圍

 

3. GLOSSARY AND DEFINITIONS

 

術(shù)語(yǔ)和定義

 

4. CONSIDERATIONS FOR QUALIFICATION UPON PURCHASING

 

采購(gòu)的確認(rèn)考慮

 

5. INITIAL QUALIFICATION

 

首次確認(rèn)

 

5.1 Qualification parameters

 

確認(rèn)參數(shù)

 

6. PERIODICAL QUALIFICATION

 

定期確認(rèn)

 

 6.1 Qualification procedure

 

確認(rèn)程序

 

 6.2 Frequency of qualification

 

確認(rèn)頻率

 

 6.3 Qualification records

 

確認(rèn)記錄

 

7. IN-USE QUALIFICATION

 

使用過(guò)程中的確認(rèn)

 

8. PROCEDURES FOR QUALIFICATION OF ANALYTICAL COLUMNS

 

色譜柱的確認(rèn)程序

 

9. REFERENCES

 

參考文獻(xiàn)

 

APPENDIX 1: EXAMPLES FOR QUALIFICATION OF ANALYTICAL COLUMNS FOR LC

 

附錄1：液相色譜柱確認(rèn)示例

 

APPENDIX 2 EXAMPLES FOR THE QUALIFICATION OF ANALYTICAL COLUMNS FOR GAS CHROMATOGRAPHY

 

附錄 2 ：氣相色譜柱確認(rèn)示例

 

1.INTRODUCTION

 

介紹

 

The present document outlines the general principles for the qualification of analytical columns used within OMCLs. Analytical columns are considered to be equipment, and as an essential part of the chromatographic system (Ph. Eur. Chapters 2.2.28, 2.2.29), they can influence the results obtained (ISO/IEC 17025:2017, Chapter 6.4 Equipment, point 6.4.1). For this reason, the qualification of analytical columns should be carried out whenever considered necessary by the OMCL.

 

本文件概述了 OMCL 中使用的分析用色譜柱確認(rèn)的一般原則。色譜柱被認(rèn)為是設(shè)備，作為色譜系統(tǒng)的重要組成部分，它們會(huì)影響分析結(jié)果（ISO/IEC 17025：2017，第 6.4 章設(shè)備，第 6.4.1 點(diǎn)）。因此，OMCL 認(rèn)為必要時(shí)應(yīng)進(jìn)行色譜柱的確認(rèn)。

 

The OMCL is responsible for defining a suitable qualification scheme for use during the life cycle of the column, depending, for example, on the intended purpose and the frequency of use.

 

OMCL 負(fù)責(zé)確定在色譜柱生命周期內(nèi)使用的合適確認(rèn)方案，例如，根據(jù)預(yù)期目的和使用頻率。

 

2.SCOPE

 

范圍

 

This document describes the requirements and general criteria for the qualification of analytical columns used in Liquid Chromatography (LC, UHPLC) and Gas Chromato-graphy (GC) procedures.

 

本文件介紹了液相色譜（LC、UHPLC）和氣相色譜（GC）程序中使用的分析用色譜柱的確認(rèn)要求和一般標(biāo)準(zhǔn)。

 

It can be used as guidance by OMCLs when planning, performing and documenting the qualification process, upon receipt and during the life cycle of analytical columns.

 

OMCL 在規(guī)劃、執(zhí)行和記錄確認(rèn)過(guò)程時(shí)，在收到色譜柱時(shí)以及在色譜柱的生命周期中，都可以將其用作指導(dǎo)。

 

Exemplary procedures provided in Annexes 1 and 2 have non-binding character. They can be helpful when carrying out the required qualification. Nevertheless, it is left to the professional judgment and background experience of each OMCL to apply the most suitable procedure, in order to prove that the analytical columns are suitable for their intended use.

 

附錄 1 和 2 中提供的示例程序具有非約束性。在執(zhí)行所需的確認(rèn)時(shí)，他們會(huì)有所幫助。然而，每個(gè) OMCL 的專業(yè)判斷和背景經(jīng)驗(yàn)都有責(zé)任應(yīng)用最合適的程序，以證明分析用色譜柱適合其預(yù)期用途。

 

3. GLOSSARY AND DEFINITIONS

 

術(shù)語(yǔ)

 

The terminology used in this document is consistent with that used in Ph. Eur. Chapter 2.2.46 “Chromatographic separation techniques”.

 

本文件中使用的術(shù)語(yǔ)與歐洲藥典第2.2.46 章“色譜分離技術(shù)”中使用的術(shù)語(yǔ)一致。

 

4.CONSIDERATIONS FOR QUALIFICATION UPON PURCHASING

 

采購(gòu)確認(rèn)的注意事項(xiàng)

 

Incoming columns shall be verified for physical damage due to shipping, for compliance with the purchase order and for completeness of the documentation.

 

應(yīng)確認(rèn)到貨色譜柱是否因運(yùn)輸而造成物理?yè)p壞、是否符合采購(gòu)訂單以及文件的完整性。

 

The OMCL shall retain records related to the management of columns for the applicable requirements described in ISO/IEC 17025:2017 clause 6.4.13.

 

應(yīng)根據(jù) ISO/IEC 17025：2017第 6.4.13 條中描述的適用要求保留與色譜柱的管理相關(guān)的記錄。

 

5.INITIAL QUALIFICATION

 

初始確認(rèn)

 

The analytical column shall be verified upon receipt or before the first use by checking the documentation (e.g. certificate of analysis) or by performing qualification of the column according to a pre-defined procedure.

 

分析用色譜柱應(yīng)在收到時(shí)或首次使用前通過(guò)檢查文件（例如COA）或根據(jù)預(yù)定的程序?qū)ιV柱進(jìn)行確認(rèn)。

 

Verification/qualification shall be documented (including, e.g. date of verification/qualification, reference to the procedure for qualification, reference materials or reagents used, results, chromatographic equipment used, pass/fail conclusion, etc.). This record can be used to make a complaint in cases where the column does not comply with the manufacturer’s specification.

 

驗(yàn)證/確認(rèn)應(yīng)有記錄（包括驗(yàn)證/確認(rèn)日期、確認(rèn)程序引用、使用的標(biāo)準(zhǔn)物質(zhì)或試劑、結(jié)果、使用的色譜設(shè)備、通過(guò)/失敗結(jié)論等）。此記錄可用于在色譜柱不符合制造商標(biāo)準(zhǔn)時(shí)進(jìn)行投訴。

 

5.1 Qualification parameters

 

確認(rèn)參數(shù)

 

It is the responsibility of the OMCL to choose the most appropriate procedure, parameters and acceptance criteria. These should be appropriate to the intended use of the column. These parameters can include resolution, symmetry factor, theoretical plates, etc. Some typical limits are given as examples in Annexes 1 and 2.

 

OMCL 有責(zé)任選擇最合適的程序、參數(shù)和接受標(biāo)準(zhǔn)。它們應(yīng)適合色譜柱的預(yù)期用途。這些參數(shù)可以包括分離度、對(duì)稱因子、理論踏板等。附件1 和附件 2 中給出了一些典型的限度標(biāo)準(zhǔn)作為示例。

 

6. PERIODICAL QUALIFICATION

 

定期確認(rèn)

 

The qualification of the columns can be performed periodically using the same test compounds/procedure. A systematic record of the qualification results should be maintained in the laboratory.

 

可以使用相同的測(cè)試化合物/程序定期進(jìn)行色譜柱的確認(rèn)。確認(rèn)結(jié)果的系統(tǒng)記錄應(yīng)在實(shí)驗(yàn)室中保存。

 

6.1 Qualification procedure

 

確認(rèn)程序

 

At least one of the procedures chosen for initial qualification can be applied for periodical qualification. The first chromatogram obtained with a new column in the laboratory can serve as a reference of column performance at the initial time point and used as a reference for subsequent verifications. Slight variations can be observed on chromatograms due to different LC or GC configuration of the equipment (e.g. dead volumes), operating environment, system electronics, etc. These can be taken into consideration whenever the acceptance criteria are set in-house.

 

至少可用初始確認(rèn)的程序進(jìn)行定期確認(rèn)。在實(shí)驗(yàn)室中使用新色譜柱獲得的第一張色譜圖可以作為該色譜柱初始性能的參考，并作為后續(xù)驗(yàn)證的參考。由于不同 LC 或GC 的設(shè)備配置（例如死體積）、運(yùn)行環(huán)境、系統(tǒng)電子元件等，色譜圖上可能會(huì)觀察到細(xì)微的不同。當(dāng)設(shè)定內(nèi)控接受標(biāo)準(zhǔn)時(shí)，可以考慮這些因素。

 

6.2 Frequency of qualification

 

確認(rèn)頻率

 

The laboratory can define and document the frequency of qualification whenever periodic qualification is considered appropriate and useful. The frequency depends on the use of the column (e.g. routine or “spot” analysis). For instance, a qualification according to section 5 (above) could be performed at fixed time intervals (e.g. once a year) or depending on the extent of use, e.g. after a defined number of injections.

 

當(dāng)認(rèn)為定期確認(rèn)適當(dāng)和有用時(shí)，實(shí)驗(yàn)室可以定義和記錄確認(rèn)頻率。頻率取決于色譜柱的使用情況（例如日常或“點(diǎn)”分析）。例如，根據(jù)第5 節(jié)（上文）的確認(rèn)可以按固定的時(shí)間間隔（例如每年一次）進(jìn)行，也可以根據(jù)使用程度進(jìn)行，例如在規(guī)定的進(jìn)樣次數(shù)后進(jìn)行。

 

6.3 Qualification records

 

確認(rèn)記錄

 

A record of the qualification results can help the user to monitor the column performance over time and inform the decision to discard it. A column is considered suitable for the intended use when the acceptance/system suitability criteria are met.

 

確認(rèn)結(jié)果的記錄可以幫助用戶監(jiān)測(cè)色譜柱性能隨時(shí)間的變化，并告知是否需要丟棄該色譜柱。當(dāng)符合接受/系統(tǒng)適用性標(biāo)準(zhǔn)時(shí)，色譜柱被認(rèn)為適合預(yù)期用途。

 

7. IN-USE QUALIFICATION

 

使用過(guò)程中的確認(rèn)

 

In-use qualification corresponds to the system suitability test for the method used. It shall be performed on a regular basis before each test and/or during the sequence of injections. In cases where the system suitability criteria are not met, the qualification of the column can be performed, to verify the consistency with the initial performance.

 

使用過(guò)程中的確認(rèn)對(duì)應(yīng)于所用方法的系統(tǒng)適用性測(cè)試。應(yīng)在每次測(cè)試前和/或在序列進(jìn)樣期間定期進(jìn)行。一旦不符合系統(tǒng)適應(yīng)性標(biāo)準(zhǔn)，可以執(zhí)行色譜柱確認(rèn)，以驗(yàn)證與初始性能的一致性。

 

The analytical procedure (e.g. mobile phase used) and the number of samples injected can contribute to the degradation of the stationary phase. The information related to the tested samples and column usage/storage conditions shall be traceable in the records (for example: samples analysed and matrix for finished products, chromatography conditions (mobile phase, temperature, pH value…).

 

分析程序（例如所使用的流動(dòng)相）和進(jìn)樣的樣品數(shù)量會(huì)導(dǎo)致固定相降解。與測(cè)試樣品和色譜柱使用/儲(chǔ)存條件相關(guān)的信息應(yīng)在記錄中可追溯（例如：分析的樣品和成品基質(zhì)、色譜條件（流動(dòng)相、溫度、pH 值......

 

8. PROCEDURES FOR QUALIFICATION OF ANALYTICAL COLUMNS

 

分析用色譜柱的確認(rèn)程序

 

Qualification of column performance can be done using one or more of the following approaches:

 

可以使用以下一種或多種方法對(duì)色譜柱性能進(jìn)行驗(yàn)證：

 

a) The column can be tested under the same conditions described in the quality control leaflet provided by the manufacturer. The same parameters should be checked and the results should be compared with the manufacturer’s results. Alternatively, other test mixtures may be used.

 

該色譜柱可以在制造商提供的質(zhì)量控制手冊(cè)中描述的相同條件下進(jìn)行測(cè)試。應(yīng)檢查相同的參數(shù)，并將結(jié)果與制造商的結(jié)果進(jìn)行比較。或者，可以使用其他測(cè)試混合物。

 

b)If the column is used only for specific test methods, it might be appropriate to perform the qualification with the system suitability test described for the test method.

 

如果該色譜柱僅用于特定的測(cè)試方法，則可能適合使用針對(duì)該測(cè)試方法所描述的系統(tǒng)適應(yīng)性測(cè)試進(jìn)行確認(rèn)。

 

c)Columns with similar stationary phases can be qualified using a general test mixture/procedure.

 

具有相似固定相的色譜柱可以使用通用測(cè)試混合物/程序進(jìn)行確認(rèn)。

 

Most of the examples given below in Annexes 1 and 2 are qualification procedures provided by manufacturers.

 

下面附件 1 和 2 中給出的示例是大多數(shù)制造商提供的確認(rèn)程序。

 

The parameters tested for the qualification of the column should be calculated and reported as defined by Ph. Eur. Chapter 2.2.46. and the results used for verification of the column performance.

 

應(yīng)按照歐洲藥典第2.2.46 章的規(guī)定計(jì)算和報(bào)告用于色譜柱確認(rèn)的參數(shù)。以及用于確認(rèn)色譜柱性能的結(jié)果。

 

Consider any differences that might occur between the parameters defined in the manufacturer specification or instrument default calculations and the requirements of Ph. Eur. Chapter 2.2.46. (Note: the tailing factor calculated by the instrument software is quite often USP tailing by default).

 

考慮制造商標(biāo)準(zhǔn)或儀器默認(rèn)計(jì)算中定義的參數(shù)與歐洲藥典第2.2.46 章的要求之間可能出現(xiàn)的任何差異。（注意：默認(rèn)情況下，儀器軟件計(jì)算的拖尾因子通常是USP 拖尾）。

 

9.REFERENCES

 

參考文獻(xiàn)

 

1)ISO/IEC 17025:2017 General requirements for the competence of testing and calibration laboratories.

 

2)Ph. Eur. Chapter 2.2.28. “Gas chromatography”.

 

3) Ph. Eur. Chapter 2.2.29 “Liquid chromatography”.

 

4) Ph. Eur. Chapter 2.2.46 “Chromatographic separation techniques”.

 

5)Column performance test mixture for liquid chromatography - standard reference material 870. NIST.

 

6) HPLC column classification. USP Pharmacopeia Forum, Vol. 31(2).

 

APPENDIX 1

 

附錄1

 

TABLE 1: EXAMPLES FOR QUALIFICATION OF ANALYTICAL COLUMNS FOR LC

 

表 1：用于 LC 的分析用色譜柱的確認(rèn)示例

 

The chromatographic conditions provided below apply to a column size of 250 mm (length) × 4.6 mm (diameter). These examples are also applicable for qualification of superficially porous particle (SPP) columns. When a column with other dimensions or SPP is used, the chromatographic conditions should be adjusted according to Ph. Eur. chapter 2.2.46.

 

下面提供的色譜條件適用于250 mm（長(zhǎng)度）× 4.6 mm（直徑）的色譜柱尺寸。這些示例也適用于表面多孔顆粒（SPP）色譜柱的確認(rèn)。當(dāng)使用其他尺寸或SPP 的色譜柱時(shí)，應(yīng)根據(jù)歐洲藥典第2.2.46 章調(diào)整色譜條件。

 

 

 

 

APPENDIX 2

 

附錄2

 

TABLE 1: EXAMPLES FOR THE QUALIFICATION OF ANALYTICAL COLUMNS FOR GAS CHROMATOGRAPHY

 

表 1：氣相色譜柱的確認(rèn)示例

 

 

 

 

Plate number

 

塔板數(shù)

 

The column performance may be calculated for a given component as the plate number (also referred to as number of theoretical plates).

 

對(duì)于給定組分，色譜柱性能可以用塔板數(shù)（也稱為理論塔板數(shù)）來(lái)計(jì)算。

 

This parameter is very useful for comparisons of GC columns. Table 2 below represents the requirements for the average column performance, given in plates/metre, according to the internal diameter and polarity of the phase.

 

此參數(shù)對(duì)于比較GC 色譜柱非常有用。下表2 顯示了根據(jù)固定相的內(nèi)徑和極性對(duì)平均色譜柱性能的要求，以板/米為單位。

 

Table 2. Comparison of average efficiency by phase polarity and internal diameter.

 

表 2.按相極性和內(nèi)徑比較平均效率。