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近日，EDQM-OMCL發(fā)布了新的《氣相色譜儀的確認(rèn)》指南。該指南包含了實(shí)驗(yàn)室氣相色譜儀的定期儀器檢查、使用中儀器的檢查的建議及相關(guān)典型接受限度，針對(duì)氣相色譜儀的定期檢查，指南給出了進(jìn)樣口泄漏測試、進(jìn)樣口壓力 / 流量準(zhǔn)確性及穩(wěn)定性、氣相色譜進(jìn)樣重復(fù)性、進(jìn)樣口溫度準(zhǔn)確性及穩(wěn)定性、進(jìn)樣口殘留、頂空進(jìn)樣重復(fù)性、樣品瓶加熱器溫度、柱箱、柱箱溫度特性重復(fù)性、火焰離子化檢測器線性、響應(yīng)穩(wěn)定性、噪聲與漂移的測試實(shí)例及其相關(guān)限度。

EDQM 儀器確認(rèn)指南將儀器的確認(rèn)分為四個(gè)級(jí)別（步驟）：

LEVEL I 選擇儀器和儀器供應(yīng)商：這一級(jí)別涉及到儀器采購的初步階段，包括確定儀器采購目的、類型 / 型號(hào)要求、供應(yīng)商要求等。設(shè)計(jì)確認(rèn)的內(nèi)容和活動(dòng)必須有記錄，并與儀器檔案一起存檔。

LEVEL II 儀器安裝和使用前驗(yàn)證：這一級(jí)別主要關(guān)注儀器在實(shí)驗(yàn)室環(huán)境下的正確安裝，并確保實(shí)驗(yàn)室的各項(xiàng)條件能滿足儀器安裝的要求。安裝確認(rèn)的內(nèi)容和活動(dòng)必須有記錄，并與儀器檔案一起存檔。

LEVEL III 儀器定期核查：這一級(jí)別涉及到儀器的周期性校準(zhǔn)和檢查，以確保儀器在使用過程中持續(xù)滿足規(guī)定的性能標(biāo)準(zhǔn)。

LEVEL IV 儀器使用中核查：這一級(jí)別涉及到在儀器使用過程中進(jìn)行的核查，以確保儀器性能持續(xù)符合檢驗(yàn)要求。

氣相色譜儀的定期檢查：
針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限值

使用中儀器的檢查：

針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限值

 

該指南翻譯如下：

 

QUALIFICATION OF GC EQUIPMENT
氣相色譜（GC）設(shè)備的確認(rèn)

CONTENTS目錄

INTRODUCTION.
簡介

LEVEL III. PERIODIC AND MOTIVATED INSTRUMENT CHECKS
LEVEL III. 定期及有動(dòng)機(jī)的儀器檢查
Recommendations for GC instruments with FID and related typical acceptance limits.
針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限度

LEVEL IV. IN-USE INSTRUMENT CHECKS
LEVEL IV. 使用中儀器的檢查
Recommendations for GC instruments with FID and related typical acceptance limits.
針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限度

LEVEL III. PERIODIC AND MOTIVATED INSTRUMENT CHECKS
LEVEL III. 定期及有動(dòng)機(jī)的儀器檢查
4.1. INLET SYSTEM.
進(jìn)樣系統(tǒng)
4.1.1. Injector leak test.
進(jìn)樣口泄漏測試
4.1.2. Inlet pressure/flow accuracy and stability.
進(jìn)樣口壓力 / 流量準(zhǔn)確性及穩(wěn)定性
4.1.3. Repeatability of GC injection.
氣相色譜進(jìn)樣重復(fù)性
4.1.4. Injector temperature accuracy and stability.
進(jìn)樣口溫度準(zhǔn)確性及穩(wěn)定性
4.1.5. Injector carry over.
進(jìn)樣口殘留
4.1.6. Repeatability of headspace injections.
頂空進(jìn)樣重復(fù)性
4.1.7. Vial heater temperature.
樣品瓶加熱器溫度
4.2. OVEN.
柱箱
4.2.1. Repeatability of the oven temperature character stics.
柱箱溫度特性重復(fù)性
4.3. FID DETECTOR.
火焰離子化檢測器（FID）
4.3.1. FID detector linearity.
火焰離子化檢測器線性
4.3.2. Constant FID detector response.
火焰離子化檢測器響應(yīng)穩(wěn)定性
4.3.3. FID detector noise and drift.
火焰離子化檢測器噪聲與漂移

OVERALL TEST 1.
綜合測試 1

OVERALL TEST 2.
綜合測試 2

OVERALL TEST 3.
綜合測試 3

1. INTRODUCTION
簡介

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 documenting the GC equipment qualification process.
本文件是核心文件《設(shè)備確認(rèn)》的第二個(gè)附錄，在規(guī)劃、執(zhí)行和記錄氣相色譜（GC）設(shè)備確認(rèn)過程時(shí)，應(yīng)與該核心文件結(jié)合使用 。

The core document contains the general introduction and the Level I and II of qualification common to all types of instruments, and the present annex contains GC instrument - related recommendations 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.
核心文件包含針對(duì)所有類型儀器的一般介紹以及LEVEL I和LEVEL II確認(rèn)內(nèi)容，本附錄包含與氣相色譜儀器相關(guān)的、關(guān)于待檢查參數(shù)和相應(yīng)典型接受限值的建議，以及關(guān)于可用于執(zhí)行這些檢查的方法的實(shí)際示例 。

Level III (Periodic and motivated instrument calibration/checks) and IV (In - use instrument checks) qualifications must be carried out as an ISO 17025 requirement. The tests proposed in the Level III and IV of qualification are based on an overall approach, in which several parameters are checked at the same time in a controlled test procedure, to obtain information on the instrument performance (e.g., peak area precision, retention time precision, temperature programme reproducibility, etc.).
Level III（定期及有動(dòng)機(jī)的儀器校準(zhǔn) / 檢查）和Level IV（使用中儀器的檢查）確認(rèn)必須按照 ISO 17025 的要求執(zhí)行。Level III和Level IV確認(rèn)中提議的測試基于一種綜合方法，即在受控測試程序中同時(shí)檢查多個(gè)參數(shù)，以獲得有關(guān)儀器性能的信息（如峰面積精度、保留時(shí)間精度、溫度程序重復(fù)性等） 。

Nevertheless, it should be noted that it is also acceptable to check these parameters individually by using other well - defined procedures.
然而，應(yīng)注意的是，使用其他明確界定的程序單獨(dú)檢查這些參數(shù)也是可接受的 。

Requirements and (if applicable) corresponding typical acceptance limits (given in bold) should be applied, however other appropriately justified approaches are acceptable. Exemplary procedures are described in this document, however, it is the responsibility of the user carrying out the required qualification. Nevertheless, it is left to the professional judgement and background experience of each OMCL to decide on the most relevant procedures to be undertaken in order to provide evidence that their GC systems are working properly and are suitable for their intended use. If the qualification of equipment is done by the manufacturer or an external service provider, it is the responsibility of the OMCL to make sure that this is in line with the requirements set out in this guideline.
應(yīng)應(yīng)用要求以及（如適用）相應(yīng)的典型接受限值（黑體字部分），但其他經(jīng)過適當(dāng)論證的方法也是可接受的。本文件中描述了示例程序，但執(zhí)行所需確認(rèn)的責(zé)任在于用戶。不過，由各官方藥品檢驗(yàn)機(jī)構(gòu)（OMCL）根據(jù)專業(yè)判斷和背景經(jīng)驗(yàn)來決定應(yīng)采用哪些最相關(guān)的程序，以提供證據(jù)證明其氣相色譜系統(tǒng)運(yùn)行正常且適合其預(yù)期用途。如果設(shè)備確認(rèn)由制造商或外部服務(wù)提供商進(jìn)行，OMCL 有責(zé)任確保其符合本指南規(guī)定的要求 。

 

2. LEVEL II. PERIODIC AND MOTIVATED INSTRUMENT CHECKS
LEVEL II. 定期及有動(dòng)機(jī)的儀器檢查

Recommendations for GC instruments with FID and related typical acceptance limits
針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限值

 

 

3. LEVEL IV. IN-USE INSTRUMENT CHECKS
3. LEVEL IV. 使用中儀器的檢查

Recommendations for GC instruments with FID and related typical acceptance limits
針對(duì)配備火焰離子化檢測器（FID）的氣相色譜（GC）儀器的建議及相關(guān)典型接受限值

 

This is to be defined in conjunction with the target concentration of the analyte
這應(yīng)結(jié)合分析物的目標(biāo)濃度來確定
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 part of the method.
在實(shí)際樣品測定的工作條件下進(jìn)行分析時(shí)，應(yīng)檢查此處給出的所有參數(shù)。通常，為此目的制備的測試和參比溶液作為方法的一部分給出

 

4. LEVEL III. PERIODIC AND MOTIVATED INSTRUMENT CHECKSLEVEL III.

定期及有動(dòng)機(jī)的儀器檢查
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.
以下給出與氣相色譜（GC）不同模塊性能相關(guān)的幾個(gè)參數(shù)的測試實(shí)例及其相關(guān)公差限值
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”.
這些實(shí)例可被官方藥品檢驗(yàn)機(jī)構(gòu)（OMCLs）視為執(zhí)行設(shè)備確認(rèn)過程LEVEL 3（“定期及有動(dòng)機(jī)的儀器檢查” ）的可行方法
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, for example, the “Grob Test” mixture, available from different suppliers (e.g. Alltech, Sigma, Thames Restek). This commercial solution should be appropriate to the column material used.
提議進(jìn)行多項(xiàng)測試以同時(shí)檢查各種參數(shù)（綜合測試）。為了以更經(jīng)濟(jì)的方式進(jìn)行測試，可使用其他合適的溶液，例如 “Grob 測試” 混合物，可從不同供應(yīng)商處獲得（如 Alltech、Sigma、Thames Restek）。該商用溶液應(yīng)與所用的色譜柱材料相適配
It is recommended to run the overall tests by using always the same test material, exclusively dedicated to qualification purposes, to guarantee reproducible conditions.
建議始終使用專門用于確認(rèn)目的的相同測試材料進(jìn)行綜合測試，以確保條件可重復(fù)
It is recommended to run the overall tests by using always the same test column, exclusively dedicated to qualification purposes, to guarantee reproducible conditions.建議始終使用專門用于確認(rèn)目的的同一根測試色譜柱來進(jìn)行綜合測試，以確保條件可重復(fù) 
4.1. INLET SYSTEM4.1 進(jìn)樣系統(tǒng)
The following tests are proposed for the periodic and motivated check of the GC Inlet System.以下測試用于對(duì)氣相色譜（GC）進(jìn)樣系統(tǒng)進(jìn)行定期和有動(dòng)機(jī)的檢查。
4.1.1. Injector leak test4.1.1 進(jìn)樣口泄漏測試
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.若儀器制造商未作其他規(guī)定，泄漏測試應(yīng)按照儀器手冊中規(guī)定的程序，或儀器內(nèi)置的自動(dòng)泄漏檢查程序進(jìn)行。
Otherwise use the test described below:否則，使用以下測試方法：
Disconnect the column from the injector and close the injector outlet with a sealed cap.將色譜柱與進(jìn)樣口斷開，并用密封帽封閉進(jìn)樣口出口。
Close the septum purge and the bypass.關(guān)閉隔墊吹掃和旁通。
Adjust the flow and pressure controller to the maximal possible value of the pressure gauge.將流量和壓力控制器調(diào)節(jié)至壓力表的最大可能值。
Adjust the flow controller to zero.將流量控制器調(diào)至零。
Read the pressure after 1 minute and record the value.1 分鐘后讀取壓力并記錄數(shù)值。Record the pressure after 5 minutes.5 分鐘后記錄壓力。
Limits限值
Pressure drop ≤ 15 kPa within 5 minutes.5 分鐘內(nèi)壓降≤15 千帕。
4.1.2. Inlet pressure/flow accuracy and stability4.1.2 進(jìn)樣口壓力 / 流量準(zhǔn)確性和穩(wěn)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.直接測量這些參數(shù)被認(rèn)為不切實(shí)際或無必要，但流量 / 壓力的最佳條件可通過綜合測試 1 進(jìn)行驗(yàn)證。
Limits: refer to overall test 1.限值：參見綜合測試 1。
4.1.3. Repeatability of GC injection4.1.3 氣相色譜進(jìn)樣重復(fù)性
The verification of this parameter is covered by the overall test 1.該參數(shù)的驗(yàn)證包含在綜合測試 1 中。
This test is to be performed in both split and split less mode.本測試需在分流和不分流模式下均進(jìn)行。
Limits: refer to overall test 1.限值：參見綜合測試 1。
4.1.4. Injector temperature accuracy and stability4.1.4 進(jìn)樣口溫度準(zhǔn)確性和穩(wěn)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.由于在不打開和改造系統(tǒng)的情況下無法可靠測量溫度，且在該模塊內(nèi)插入探針存在困難，該參數(shù)的驗(yàn)證被認(rèn)為包含在綜合測試 2 中。
Limits: refer to overall test 2.限值：參見綜合測試 2。
4.1.5. Injector carry over4.1.5 進(jìn)樣口殘留
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 (or analytes) in the linearity solutions.在按遞增順序注入用于火焰離子化檢測器（FID）線性測試的溶液后，注入空白樣品，并測量與線性測試溶液中主要峰（或分析物）對(duì)應(yīng)的峰。
The verification of this parameter is covered by the overall test 3.該參數(shù)的驗(yàn)證包含在綜合測試 3 中。
Limits: refer to overall test 3.限值：參見綜合測試 3。
HEAD SPACE INJECTORS頂空進(jìn)樣器
4.1.6. Repeatability of headspace injections4.1.6 頂空進(jìn)樣重復(fù)性
Method.方法
The GC - HS operating conditions below are provided as an example, adjustments may be needed depending on the equipment used.以下氣相色譜 - 頂空（GC - HS ）操作條件為示例，可能需要根據(jù)所用設(shè)備進(jìn)行調(diào)整。
Test solution: 0.5% ethanol in water R (V/V)測試溶液：含 0.5% 乙醇的水（R ）溶液（體積 / 體積 ）
GC - Settings:氣相色譜設(shè)置：
Column: 95% Dimethyl / 5% diphenylpoly siloxane 30 m × 0.25 μm, 0.25 mm (HP - 5 was found suitable)色譜柱：95% 二甲基 / 5% 二苯基聚硅氧烷，30 米 ×0.25 微米，0.25 毫米（發(fā)現(xiàn) HP - 5 柱適用 ）
Carrier gas: Helium載氣：氦氣
Column Flow: 1.2 ml/min柱流速：1.2 毫升 / 分鐘
Injector temperature: 200 °C進(jìn)樣口溫度：200℃
Split ratio: 1:50分流比：1:50
Oven temperature: 40 °C isotherm柱箱溫度：40℃恒溫
Detector temperature: 250 °C檢測器溫度：250℃
Run time: 1.5 folds the retention time of the main peak運(yùn)行時(shí)間：主峰保留時(shí)間的 1.5 倍
Retention time: about 2.2 min保留時(shí)間：約 2.2 分鐘
Headspace - Settings:頂空設(shè)置：
Carrier pressure: 9.9 psi載氣壓力：9.9 磅力 / 平方英寸
Vial pressure: 14.2 psi樣品瓶壓力：14.2 磅力 / 平方英寸
Shake: low振蕩：低強(qiáng)度
Oven Temperature: 80 °Coven（頂空爐）溫度：80℃
Loop Temperature: 90 °C定量環(huán)溫度：90℃
Transfer line Temperature: 100 °C傳輸線溫度：100℃
Vial size: 20 mL樣品瓶規(guī)格：20 毫升
Volume of sample solution/vial: 5 mL每瓶樣品溶液體積：5 毫升
Vial Equilibration Time: 15.0 min樣品瓶平衡時(shí)間：15.0 分鐘
Inject Time: 1.0 min進(jìn)樣時(shí)間：1.0 分鐘
Loop Equilibration Time: 0.1 min定量環(huán)平衡時(shí)間：0.1 分鐘
Loop Fill Time: 0.5 min定量環(huán)填充時(shí)間：0.5 分鐘
Vial Pressurization Time: 0.08 min樣品瓶加壓時(shí)間：0.08 分鐘
Carry out 6 consecutive injections of the test solution and calculate the RSD of the different peak areas and retention times.對(duì)測試溶液連續(xù)進(jìn)樣 6 次，計(jì)算不同峰面積和保留時(shí)間的相對(duì)標(biāo)準(zhǔn)偏差（RSD ）。
Limits:限值：
Peak areas: the RSD should be ≤ 5.0%峰面積：相對(duì)標(biāo)準(zhǔn)偏差應(yīng)≤5.0%
Retention time: the RSD should be ≤ 2.0%保留時(shí)間：相對(duì)標(biāo)準(zhǔn)偏差應(yīng)≤2.0%
4.1.7. Vial heater temperature4.1.7 樣品瓶加熱器溫度
The heater temperatures are to be set up at values which depend on the operating conditions of the methods applied.加熱器溫度應(yīng)根據(jù)所采用方法的操作條件設(shè)定相應(yīng)數(shù)值。
Suitable calibrated temperature devices are to be used.應(yīng)使用合適的經(jīng)校準(zhǔn)的溫度測量設(shè)備。
Put the calibrated device in the oven of the head space compartment. Set the temperature at the required values. When equilibration is achieved, record the value displayed on the calibrated device.將經(jīng)校準(zhǔn)的設(shè)備放入頂空進(jìn)樣器的爐腔中。將溫度設(shè)定為所需數(shù)值。達(dá)到平衡后，記錄經(jīng)校準(zhǔn)設(shè)備上顯示的數(shù)值。
Limits: ± 4 °C from set point限值：與設(shè)定點(diǎn)的偏差為 ±4℃
4.2. OVEN4.2 柱箱
4.2.1. Repeatability of the oven temperature characteristics4.2.1 柱箱溫度特性的重復(fù)性
Due to the fact that the temperature cannot be reliably measured without opening and modifying the 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.由于在不打開和改變系統(tǒng)條件的情況下無法可靠測量溫度，而且即使在柱箱內(nèi)插入一個(gè)探頭，其位置也無法反映所有點(diǎn)的實(shí)際溫度情況，所以該參數(shù)的驗(yàn)證包含在綜合測試 2A 和 2B 中。
Limits: refer to overall test 2.限值：參見綜合測試 2
4.3. FID DETECTOR4.3 火焰離子化檢測器（FID）
The following tests are proposed for the periodic and motivated check of the GC FID detector.以下測試用于對(duì)氣相色譜火焰離子化檢測器進(jìn)行定期和有動(dòng)機(jī)的檢查
4.3.1. FID detector linearity4.3.1 火焰離子化檢測器的線性
Increasing amounts of analyte are injected and a linear response should be obtained.注入遞增量的分析物，應(yīng)獲得線性響應(yīng)。
The verification of this parameter is covered by the overall test 3.該參數(shù)的驗(yàn)證包含在綜合測試 3 中。
Limits: refer to overall test 3.限值：參見綜合測試 3
4.3.2. Constant FID detector response4.3.2 火焰離子化檢測器響應(yīng)的穩(wěn)定性
The proper and reproducible functioning of the FID can be demonstrated by checking the peak areas obtained from a pre - defined standard solution.通過檢查從預(yù)定義標(biāo)準(zhǔn)溶液中獲得的峰面積，可證明火焰離子化檢測器功能正常且具有可重復(fù)性。
The verification of this parameter is covered by the overall test 1 or 2.該參數(shù)的驗(yàn)證包含在綜合測試 1 或 2 中。
Limits: refer to overall test 1 or 2.限值：參見綜合測試 1 或 2
4.3.3. FID detector noise and drift4.3.3 火焰離子化檢測器的噪聲和漂移
If the instrument has a built - in automatic system for the verification of the noise and drift, follow the manufacturer’s instructions and apply the defined acceptance criteria. Otherwise, use the test described below:如果儀器配有用于驗(yàn)證噪聲和漂移的內(nèi)置自動(dòng)系統(tǒng)，按照制造商的說明操作并應(yīng)用規(guī)定的接受標(biāo)準(zhǔn)。否則，使用以下測試方法：
Settings:設(shè)置：
Column installed安裝色譜柱
Suitable flow, depending on column length/diameter合適的流量，取決于色譜柱長度 / 直徑
No injection不進(jìn)樣
Oven temperature: 40 °C柱箱溫度：40℃
Detector is on and heated at working temperature (270 - 300 °C)檢測器開啟并在工作溫度（270 - 300℃ ）下加熱
Method方法
After stabilisation of the system, record the signal for 15 minutes.系統(tǒng)穩(wěn)定后，記錄信號(hào) 15 分鐘。
Noise: evaluate 10 periods of 1 minute and calculate the mean value.噪聲：評(píng)估 10 個(gè) 1 分鐘的周期并計(jì)算平均值。
Drift: evaluate the slope of the baseline over the 15 minutes.漂移：評(píng)估 15 分鐘內(nèi)基線的斜率。
Limits:限值：
The acceptance criteria for these parameters have to be chosen in accordance with the instrument vendor’s instructions and the intended use of the instrument. If no instructions are given, the user has to pre - define these acceptance criteria by taking into account the previous experience and the intended use of the instrument.這些參數(shù)的接受標(biāo)準(zhǔn)必須根據(jù)儀器供應(yīng)商的說明以及儀器的預(yù)期用途來選定。如果沒有說明，用戶必須考慮以往經(jīng)驗(yàn)和儀器預(yù)期用途來預(yù)先定義這些接受標(biāo)準(zhǔn)。
No fixed values can be pre - defined in this guideline due to the high variety of integration systems used and consequently the acceptance criteria may be expressed in different units (voltage, current, arbitrary units per time).由于所用積分系統(tǒng)種類繁多，本指南無法預(yù)先定義固定值，因此接受標(biāo)準(zhǔn)可能以不同單位（電壓、電流、每時(shí)間任意單位 ）表示。

5. OVERALL TEST 15. 綜合測試 1
The overall test 1 covers the following parameters:綜合測試 1 涵蓋以下參數(shù)：
Pressure/flow accuracy and stability in the inlet system; Retention time repeatability進(jìn)樣系統(tǒng)中壓力 / 流量的準(zhǔn)確性和穩(wěn)定性；保留時(shí)間重復(fù)性
Repeatability of injection: peak area precision進(jìn)樣重復(fù)性：峰面積精度
In split mode分流模式
In split less mode不分流模式
The test may be combined with overall test 3.本測試可與綜合測試 3 結(jié)合進(jìn)行。
Split mode:分流模式：
Test solution:測試溶液：
1 - octanol in n - hexane 1% (V/V).正己烷中 1%（體積 / 體積 ）的 1 - 辛醇
Settings:設(shè)置：
Column: 100% Dimethylpolysiloxane 30m x 0.32mm ID x 0.25μm film (SPB - 1 was found suitable)色譜柱：100% 二甲基聚硅氧烷，30 米 ×0.32 毫米內(nèi)徑 ×0.25 微米膜厚（發(fā)現(xiàn) SPB - 1 柱適用 ）
Carrier gas: Helium載氣：氦氣
Velocity: 25cm/sec線速度：25 厘米 / 秒
Split: 1:100分流比：1:100
Injection: 1μl進(jìn)樣量：1 微升
Injector temperature: 220 °C進(jìn)樣口溫度：220℃
Oven temperature: 100 °C isotherm柱箱溫度：100℃恒溫
Detector temperature: 300 °C檢測器溫度：300℃
Run time: 1.5 folds the retention time of the main peak運(yùn)行時(shí)間：主峰保留時(shí)間的 1.5 倍
Retention time of 1 - octanol: about 5 min1 - 辛醇的保留時(shí)間：約 5 分鐘
Split less mode:不分流模式：
Stock solution: 1 - octanol in n - hexane 1% (V/V)儲(chǔ)備溶液：正己烷中 1%（體積 / 體積）的 1 - 辛醇
Test solution: Dilute 10 ml of the stock solution with n - hexane to 100 ml (corresponds to 1μl/ml of 1 - octanol in n - hexane)測試溶液：取 10 毫升儲(chǔ)備溶液，用正己烷稀釋至 100 毫升（相當(dāng)于正己烷中 1 - 辛醇濃度為 1 微升 / 毫升 ）
Settings:設(shè)置：
Column: 100% Dimethylpolysiloxane 30m, 0.32mm ID, 0.25μm film (SPB - 1 was found suitable)色譜柱100% 二甲基聚硅氧烷，30 米，內(nèi)徑 0.32 毫米，膜厚 0.25 微米（發(fā)現(xiàn) SPB - 1 柱適用 ）
Carrier: Helium載氣：氦氣
Velocity: 30cm/sec線速度：30 厘米 / 秒
Split less injection: purge valve closed during 2 min不分流進(jìn)樣：吹掃閥關(guān)閉 2 分鐘
Injection: 0.2μl of the test solution進(jìn)樣：0.2 微升測試溶液
Injector Temperature: 220 °C進(jìn)樣口溫度：220℃
Oven Temperature: Initial 60 °C for 4 min, 15 °C/min, up to 135 °C, final time 1min柱箱溫度：初始 60℃保持 4 分鐘，以 15℃/ 分鐘升溫至 135℃，最終保持 1 分鐘

Detector Temperature: 300 °C檢測器溫度：300℃
Runtime: 1.5 folds the retention time of the main peak運(yùn)行時(shí)間：主峰保留時(shí)間的 1.5 倍
Retention time of 1 - octanol: about 8 min1 - 辛醇的保留時(shí)間：約 8 分鐘
Method:方法：
Carry out 6 consecutive injections of the test solution and calculate the RSD of the different peak areas and retention times.對(duì)測試溶液連續(xù)進(jìn)樣 6 次，計(jì)算不同峰面積和保留時(shí)間的相對(duì)標(biāo)準(zhǔn)偏差（RSD ）。
Limits:限值：
Retention time repeatability: the RSD of the retention times should be ≤ 2.0%保留時(shí)間重復(fù)性：保留時(shí)間的相對(duì)標(biāo)準(zhǔn)偏差應(yīng)≤2.0%
Peak area precision (split and split - less mode): the RSD of the peak areas should be ≤ 3.0%峰面積精度（分流和不分流模式 ）：峰面積的相對(duì)標(biāo)準(zhǔn)偏差應(yīng)≤3.0%

6. OVERALL TEST 26. 綜合測試 2
The overall test 2 covers the following parameters:綜合測試 2 涵蓋以下參數(shù)：
Injector, oven and detector temperature accuracy and stability: retention time repeatability進(jìn)樣口、柱箱和檢測器溫度準(zhǔn)確性和穩(wěn)定性：保留時(shí)間重復(fù)性
Two alternative tests are proposed:提議兩種替代測試：
Overall test 2A綜合測試 2A
Test solution:測試溶液：
0.03 ml 1 - octanol0.03 毫升 1 - 辛醇
0.03 ml 2 - butanone0.03 毫升 2 - 丁酮
0.035 ml 2,6 - dimethylanilin0.035 毫升 2,6 - 二甲基苯胺
0.035 ml n - tridecane0.035 毫升正十三烷
0.035 ml n - tetradecane0.035 毫升正十四烷
35 mg n - eicosane35 毫克正二十烷
dissolved in 50 ml Dichloromethane溶解于 50 毫升二氯甲烷中

Settings:

設(shè)置：

Column: 100% Dimethylpolysiloxane 30m x 0.32mm ID x 0.25μm film (SPB - 1 was found suitable)色譜柱：100% 二甲基聚硅氧烷，30 米 ×0.32 毫米內(nèi)徑 ×0.25 微米膜厚（發(fā)現(xiàn) SPB - 1 柱適用 ）

Carrier gas: Helium載氣：氦氣

Velocity: 25 cm/s線速度：25 厘米 / 秒

Split: 1:100分流比：1:100

Injection volume: 1μl進(jìn)樣體積：1 微升

Injector temperature: 220 °C進(jìn)樣口溫度：220℃

Detector: FID檢測器：火焰離子化檢測器（FID ）

Detector temperature: 300 °C檢測器溫度：300℃

Gradient programme: 60 °C (4 min), 5 °C/min, 270 °C (3 min)梯度程序：60℃（保持 4 分鐘 ），以 5℃/ 分鐘升溫，270℃（保持 3 分鐘 ）

Method:

方法：

Inject the solution twice and calculate the relative retention (RR) times in relation to n - eicosane (RR = 1)
進(jìn)樣兩次，計(jì)算相對(duì)于正二十烷的相對(duì)保留（RR ）時(shí)間（正二十烷的相對(duì)保留設(shè)為 1 ）

The following table shows the approximately expected relative retention times.
下表顯示大致預(yù)期的相對(duì)保留時(shí)間。

 

Analyte分析物	1-octanol1 - 辛醇	2-octanone2 - 辛酮	2,6-dimethylaniline2,6 - 二甲基苯胺	n-tridecane正十三烷	n-tetradecane正十四烷
RRT (Relative Retention Time)相對(duì)保留時(shí)間（RRT）	0.30	0.22	0.37	0.52	0.60

Limits:限值：
The RSD of each RR from two consecutive injections should be ≤ 1.0%兩次連續(xù)兩次進(jìn)樣中，每個(gè)相對(duì)保留值（RR）的相對(duì)標(biāo)準(zhǔn)偏差（RSD）應(yīng)≤1.0%
Overall test 2B綜合測試 2B
Test Solution:測試溶液：
1.0% (m/m) n - Nonane and Hexadecane in Tetradecane.正十四烷中含 1.0%（質(zhì)量 / 質(zhì)量）的正壬烷和十六烷
Settings:設(shè)置：
Column: 100% Dimethylpolysiloxane 25m x 0.32mm ID x 0.52μm film (Ultra - 1 was found suitable)色譜柱：100% 二甲基聚硅氧烷，25 米 ×0.32 毫米內(nèi)徑 ×0.52 微米膜厚（發(fā)現(xiàn) Ultra - 1 柱適用 ）
Injection volume: 1μl進(jìn)樣體積：1 微升
Solvent: Tetradecane溶劑：正十四烷
Injection temperature: 250 °C進(jìn)樣口溫度：250℃
Gradient programme: 110 °C, 20 °C/min, 180 °C (final time: 3.5 min)梯度程序：110℃，以 20℃/ 分鐘升溫，180℃（最終保持 3.5 分鐘 ）
Detector temperature: 250 °C檢測器溫度：250℃
Injector temperature: 200 °C進(jìn)樣口溫度：200℃
Detector: FID檢測器：火焰離子化檢測器（FID ）
Flow rates: as defined by the instrument manufacturer流速：按儀器制造商規(guī)定
Split ratio: 1:15分流比：1:15
Split vent: 30 ± 3.0 ml/min分流出口流速：30±3.0 毫升 / 分鐘
Septum purge: 3 - 5 ml/min隔墊吹掃流速：3 - 5 毫升 / 分鐘
Method:方法：
Allow the system to equilibrate.使系統(tǒng)達(dá)到平衡。
Injection sequence:進(jìn)樣序列：
blank (Tetradecane)空白（正十四烷 ）
6 replicates of the test solution. Calculate the mean of the retention times and the relative standard deviation of n-Nonane and n-Hexadecane.對(duì)測試溶液進(jìn)行 6 次重復(fù)進(jìn)樣。計(jì)算正壬烷和正十六烷保留時(shí)間的平均值以及相對(duì)標(biāo)準(zhǔn)偏差。
Limits:限值：
Retention time repeatability: RSD of the peak retention times of the 6 replicates ≤ 2.0%保留時(shí)間重復(fù)性：6 次重復(fù)進(jìn)樣中峰保留時(shí)間的相對(duì)標(biāo)準(zhǔn)偏差≤2.0%
Retention time (RT) accuracy: For this example, the retention time ranges shown in the table below are proposed. Nevertheless, individual ranges should be predefined by the laboratory depending on the column used (e.g., Rt. ± 0.2 min).保留時(shí)間（RT）準(zhǔn)確性：對(duì)于本示例，建議采用下表中所示的保留時(shí)間范圍。不過，實(shí)驗(yàn)室應(yīng)根據(jù)所用色譜柱預(yù)先定義各自的范圍（例如，保留時(shí)間 ±0.2 分鐘 ）。

Compound化合物	Rt (min)保留時(shí)間（分鐘）
n-Nonane (C?)正壬烷（C?）	1.3 – 1.71.3 – 1.7
Tetradecane (C??)正十四烷（C??）	4.0 – 4.74.0 – 4.7
Hexadecane (C??)正十六烷（C??）	5.1 – 6.05.1 – 6.0

 

7. OVERALL TEST 3

7. 綜合測試 3

This test is a modified version of the overall test 1 to be used for the verification of:
本測試是綜合測試 1 的修改版，用于驗(yàn)證以下內(nèi)容：

Detector linearity: linearity of the areas recorded檢測器線性：所記錄峰面積的線性

Detector carry - over: area recorded in the blank run檢測器殘留：空白運(yùn)行中記錄的峰面積

It is described for both split and split less mode and may be combined with overall test 1.
本測試針對(duì)分流和不分流模式進(jìn)行說明，且可與綜合測試 1 結(jié)合進(jìn)行。

Split mode:

分流模式：

Test solution: 1 - octanol in n - hexane 1% (V/V)
測試溶液：正己烷中 1%（體積 / 體積 ）的 1 - 辛醇

Prepare further reference solutions by diluting the test solution as described below.
按以下方法稀釋測試溶液，制備更多參比溶液。

Settings: see overall test 1
設(shè)置：參見綜合測試 1

Injection sequence:
進(jìn)樣序列：

5.0 ml of the test solution diluted to 25.0 ml with n - hexane (2 μl/ml): 2 injections取 5.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 2 微升 / 毫升 ）：進(jìn)樣 2 次
10.0 ml of the test solution diluted to 25.0 ml with n - hexane (4 μl/ml): 2 injections取 10.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 4 微升 / 毫升 ）：進(jìn)樣 2 次
15.0 ml of the test solution diluted to 25.0 ml with n - hexane (6 μl/ml): 2 injections取 15.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 6 微升 / 毫升 ）：進(jìn)樣 2 次
20.0 ml of the test solution diluted to 25.0 ml with n - hexane (8 μl/ml): 2 injections取 20.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 8 微升 / 毫升 ）：進(jìn)樣 2 次
If combined with overall test 1 for repeatability: test solution (10 μl/ml): 6 injections若與綜合測試 1 結(jié)合進(jìn)行重復(fù)性測試：測試溶液（濃度為 10 微升 / 毫升 ）：進(jìn)樣 6 次n - hexane as blank (carry over)正己烷作為空白（用于檢測殘留 ）

Split - less mode:

不分流模式：

Stock solution: 1 - octanol in n - hexane 1% (V/V)
儲(chǔ)備溶液：正己烷中 1%（體積 / 體積 ）的 1 - 辛醇

Test solution: Dilute 10 ml of the stock solution with n - hexane to 100 ml (corresponds to 1μl/ml of 1 - octanol in n - hexane).
測試溶液：取 10 毫升儲(chǔ)備溶液，用正己烷稀釋至 100 毫升（相當(dāng)于正己烷中 1 - 辛醇濃度為 1 微升 / 毫升 ）。

Prepare further reference solutions by diluting the test solution with n - hexane.
用正己烷稀釋測試溶液，制備更多參比溶液。

Settings: see overall test 1
設(shè)置：參見綜合測試 1

Injection sequence:進(jìn)樣序列：
5.0 ml of the test solution diluted to 25.0 ml with n - hexane (0.2 μl/ml): 2 injections取 5.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 0.2 微升 / 毫升 ）：進(jìn)樣 2 次
10.0 ml of the test solution diluted to 25.0 ml with n - hexane (0.4 μl/ml): 2 injections取 10.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 0.4 微升 / 毫升 ）：進(jìn)樣 2 次
15.0 ml of the test solution diluted to 25.0 ml with n - hexane (0.6 μl/ml): 2 injections取 15.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 0.6 微升 / 毫升 ）：進(jìn)樣 2 次
20.0 ml of the test solution diluted to 25.0 ml with n - hexane (0.8 μl/ml): 2 injections取 20.0 毫升測試溶液，用正己烷稀釋至 25.0 毫升（濃度為 0.8 微升 / 毫升 ）：進(jìn)樣 2 次
if combined with overall test 1 for repeatability: test solution (1 μl/ml): 6 injections若與綜合測試 1 結(jié)合進(jìn)行重復(fù)性測試：測試溶液（濃度為 1 微升 / 毫升 ）：進(jìn)樣 6 次
n - hexane as blank (carry over)正己烷作為空白（用于檢測殘留 ）
Limits:限值：
Linearity: coefficient of correlation of the calibration line obtained with the reference solutions and the test solution: r² ≥ 0.999.線性：用參比溶液和測試溶液得到的校準(zhǔn)曲線的相關(guān)系數(shù)：r²≥0.999。
Carry - over: the percentage of the peak area corresponding to the analyte in the blank solution should be ≤ 0.2% of the peak area of this analyte in the chromatogram obtained with the solution with the highest concentration within the sequence.殘留：空白溶液中與分析物對(duì)應(yīng)的峰面積百分比，應(yīng)≤進(jìn)樣序列中最高濃度溶液的色譜圖中該分析物峰面積的 0.2%。