GC设备的确认(中英) Qualification of GC equipment

2. Peak area precision

峰面积精度

RSD

≤

3.0% unless otherwise prescribed*

RSD

≤

3.0%

，除非另有规定

3. Retention time repeatability

保留时

间的重复性

RSD

≤

2.0%

4. Sensitivity (where relevant, e.g. for

related substances tests)

灵敏度（例

如有关物质检测）

According to Ph. Eur. or MAH dossier or

validated in-house method

根据欧盟药典或

MAH

文件，或者公司内部已验证的方法

*

This is to be defined in conjunction with the target concentration of the analyte

这需要与被分析物的目标浓度联系起来确定。

All parameters given here should be checked when performing analyses

under the working

conditions

for the actual sample determinations. Normally, the test and 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该

在工作条件 下

对实际样品的测定结果进行分析时进行检查。

正常情况下，为此目的配制的供试溶液和标准溶液是作为该方法的一部分。

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PA/PH/OMCL (06) 86 DEF - OMCL Guideline on Qualification of GC equipment (Annex 2)

ANNEX I

附件

I

Level III. Periodic and motivated instrument checks

阶段

III.

对仪器的定期和专门检查

Practical examples of tests and their associated tolerance limits for several parameters related

to the performance of the different modules of a GC are presented below.

下面展示的是检测

GC

仪器不同模块性能的实际例子及其参数的误差限度。

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

”

.

OMCLs

认为这些例子可以用来 执行设备确认过程的阶段

III

“对仪器进行定期和专门检测”

。

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

“G

rob

Tes

t”

mixture,

available

from

different

suppliers

(e.g.

Alltech,

Sigma,

Thames Restek). This commercial solution should be appropriate to the column material used.

建议同时做几个测试来检测不同的参数（全面检测）。为了以更经济的方法进行检测，其他合适的

解决方法也可以使用，例如

,

“

Grob Test

”混合物，可以从不同的供应商

(

例如

, Alltech, Sigma,

Thames Restek )

处得到。

这个商业化的解决方案应该适用于使用的色谱柱材料。

It is recommended to run the overall tests by using always the same test column, exclusively

dedicated to qualification purposes, to guarantee reproducible conditions.

建议只使用专门用

于确认的同一根色谱柱来进行全面检测，以确 保条件的可重现性。

1.

INLET SYSTEM

进样系统

The following tests are proposed for the periodic and motivated check of the GC Inlet S ystem.

建议对

GC

进样系统的定 期和专门检测实施以下检测

1.1.

INJECTOR LEAK TEST

进样器密封性

(

检漏

)

检测

Method

方法

< br>:

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.

如果仪器厂家没有特别说明，密封性检测根据仪器说明书上写 的程序进行，或者仪器内的自动

泄漏检测程序进行。

Otherwise use the test described below:

否则就使用下面的检测方法

Disconnect the column from the injector and close the injector outlet with a sealed cap.

从进样器上断开色谱柱，用密封帽封住进样器出口

Close the septum purge and the bypass.

关闭隔膜和旁路

Adjust the flow and pressure controller to the maximal possible value of the pressure gauge.

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PA/PH/OMCL (06) 86 DEF - OMCL Guideline on Qualification of GC equipment (Annex 2)

调整流动和压力控制器到压力计的最大可能值

Adjust the flow controller to zero.

调整流速控制器到零

。

Read the pressure after 1 minute and record the value.

1

分钟后读压力值并记录

Record the pressure after 5 minutes.

5

分钟后记录压力值

Limits

限度

< br>:

Pressure drop

≤

15 kPa within 5 minutes. < /p>

5

分钟内压力下降

≤

15 kPa

1.2.

INLET PRESSURE/FLOW ACCURACY AND STABILITY

进气压力

/

流 速

的准确性

和稳定性

A

direct

measurement

of

these

parameters

was

not

deemed

practical

or

necessary,

but

the

optimal conditions of flow/pressure can be verified by the overall test 1.

直接测量这些参数是不实际或者不必要的，但是 流动

/

压力的最佳条件可以通过全面检测

1

来确认

。

Limits

限度

:

refer to overall test 1.

参考全面检测

1

1.3.

REPEATABILITY OF INJECTION

进样的可重现性

The verification of this parameter is covered by the overall test 1.

此参数的确认包 括在全面检测

1

中。

This test is to be performed in both split and split less mode.

本次检测在分流

(split)

和分流较少

(split less)

两种模式下都应进行。

Limits

限度

:

refer to overall test 1.

参考全面检测

1

1.4.

INJECTOR TEMPERATURE ACCURACY AND STABILITY

进样器温度的准确性和稳定性

Due

to

the

fact

that

the

temperature

cannot

be

reliably

measured

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.

由于考虑到温度在没有打开和改动系统的情况下无法可靠测量 以及把探头放入模块的难度，

此参数的确认可以涵盖在全面检测

2

中。

Limits

限度

:

refer to overall test 2.

参见全面检测

2

1.5.

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.

在注入用于检测

FID

检测器线性的溶 液后，按照浓度依次增加的顺序，进空白然后测量与线性

溶液中主峰想对应的各个峰

(

被分析物

)

。

The verification of this parameter is covered by the overall test 3.

此

参数的确认包括在全面检测

3

中。

October 2006

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