仪器确认 附件7 质谱仪确认 中英文

OMCL Network of the Council of Europe

QUALITY MANAGEMENT DOCUMENT

质量管理文件

PA/PH/OMCL (10) 86 2R

QUALIFICATION OF EQUIPMENT

仪器确认

ANNEX 7: QUALIFICATION OF MASS SPECTROMETERS

附件< /p>

7

：质谱仪的确认

Full document title and reference

文件全名和索引号

Document type

文件类型

Legislative basis

立法基础

Date of first adoption

首次发行日期

Date of original entry into force

首次执行日期

Date of entry into force of revised

document

修订后执行日期

Previous titles/other references

原文件 名

/

其它索引号

Custodian Organisation

保管机构

Concerned Network

相关网络

Qualification of Equipment

Annex 7: Qualification of mass spectrometers

PA/PH/OMCL(10)86 2R

Guideline

-

25

th

May 2011

1

st

July 2011

-

-

The present document was elaborated by the OMCL

Network/EDQM of the Council of Europe

GEON

ANNEX 7 OF THE OMCL NETWORK GUIDELINE

“QUALIFICATION OF EQUIPMENT”

OMCL

网络指南“仪器确认”附件

7

7.1: QUALIFICATION OF GAS CHROMATOGRAPHY-MASS SPECTROMETERS

WITH ELECTRON IMPACT IONIZATION (GC-EI-MS)

装 备电子碰撞电离的气相色

谱

-

质谱仪的 确认

Introduction

介绍

The present document is the first part of the 7

th

Annex of the co

re document “Qualification of

Equipment”, and it should be used in combination with it when planning, performing and

documenting the qualification process of GC-EI-MS.

本文件是核心文件“仪器确认”的第

7

个附件，在计实施和记录

GC-EI-MS

的确认过程中，

应与核心文件结合使用。

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 了介绍和适用于所有类型仪器的第一级和第二级确认用通用表格。

The present annex 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 包括与仪器相关的在第三级和第四级要检查的参数及其相关的典型可接受限度的

推荐，以 及在实施这些检查时可以采用的方法学实例。

TABLE III

表

3

Level III. Periodic and motivated instrument checks

第三级

周期性主动仪检查

Minimum requirements for GC-EI-MS

(examples)

GC-EI-MS

最低要求（举例）

Parameter to be checked

要检查的参数

Mass accuracy

质量准确性

PFTBA (FC-43) *

Or internal calibration gas

或内部校正气体

Linearity **

线性

System/instrument precision **

系统

/

仪器 精密度

*)

PFTBA (FC-43): Perfluoro-tributyl-amine (CAS NO.: 311-89-7)

Typical tolerance limits

典型允许限度

m/z = 69±

0.5

m/z = 219±

0.5

m/z = 502±

0.5

or defined masses of internal calibration gas ±

0.5

或内校气体指定的质量

±

0.5

r2 ≥0.995

≤1.0%

如果要进行定量

PFTBA(FC-43):

全氟三丁胺（

< br>CAS

号

311-89-7

）

**)

In case of quantification purposes, these parameters have to be checked.

检测，这些参数必须要检查。

TABLE IV

表四

Level IV. In-use instrument checks

第四级

在用仪器的检查

Requirements for GC-EI-MS

GC-EI-MS

的要求

Parameter to be checked

要检查的参数

As defined by the specific analysis method or

according to the Ph. Eur. Or the MAH dossier

(see example in Level IV

. Annex II)

如特定分析方法定义，或根据欧 洲药典或

MAH

档案（见第四级附件

2

的举例）

Typical tolerance limits

典型允许限度

Identified by library or with reference standard

由图谱库进行鉴别或与对照品进行对照

ANNEX I

附件

1

Level III. Periodic and motivated instrument checks

第三级

周期性主动仪器检查

This Annex contains

practical examples

of tests and their associated tolerance limits for

several parameters related to the performance of GC-EI-MS.

本附件包括了

GC-EI- MS

性能相关的几个参数的测试实例及其关联的允许限度。

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 checks”.

这些实例可以作为

OMCL

在实施第三级仪器确认过程“周期性主动仪器检查”中可以采

用的方法。

GENERAL CONSIDERATIONS

一般考虑

- GC-MS is mainly used for the identification of unknown substances or quantification of low

concentrated substances where high specificity is needed.

GC-MS

主要用于需要较高专属性 的未知物质的鉴别，或低浓度物质的定量

MASS ACCURACY

质量准确度

Materials:

材料

PFTBA (FC-43) or internal calibration gas

PFTBA(FC-43)

或内部校正气体

Method:

方法

Internal instrument check or spectrum of PFTBA (FC-43) in full scan mode

仪器内部检查或

（

FC-43

）全扫描模式光谱扫描

Limits:

限度

m/z = 69 ±

0.5

m/z = 219 ±

0.5

m/z = 502 ±

0.5

Note

: the tolerance limits for mass accuracy are only valid for quadrupole and ion trap mass

spectrometers. Instruments like Time-of-Flight (TOF) or hybrid instruments like

quadrupole-Time-of- Flight (QTOF) have a much better mass accuracy and adequate

requirements should be applied by the laboratory.

注：质量准确度的 允许限度只对四级杆和离子阱质谱仪有效。其它仪器，如飞行时间质

谱

< br>（

TOF

）

或

< br>HYBRID

仪器，

如四级杆

-

飞行时间质谱

（

QTOF

）

，

具有更好的质量准确性，

这时化验室应采用足够好的要求。

LINEARITY

线性

Materials:

材料

Stock solutions: 1-

Octanol in dichloromethane 0.2, 0.4, 0.6, 0.8, 1.0 μL/mL

贮备液：

0.2, 0.4, 0.6, 0.8, 1.0 μL/mL

正辛醇的二氯甲烷溶液

Method:

方法

2 injections of each level (injection volume: 1.0 μL)

每个水平

2

针（进样量

1.0uL

）

Limits:

限度

r? ≥ 0.995

SYSTEM/INSTRUMENT PRECISION

系统

/

仪器精密度

Materials:

材料

Stock solution: 1-

Octanol in dichloromethane 1.0 μL/mL

贮备液：

1.0 μL/mL

正辛醇的二氯甲烷溶液

Method:

方法

6 injections

(injection volume: 1.0 μL)

6

针（进样量：

1.0uL

）

Limits (minimum requirement):

限度（最低要求）

RSD ≤ 10.0% (without internal standard

没有内控标准

)