气相再确认方案.docx

1、气相再确认方案PRE-EXECUTION APPROVAL执行前批准DEPARTMENT部门PRINT NAME/TITLE姓名/职务SIGNATURE 签名DATE日期SYSTEM OWNER系统所属部门QA质量保证部OQ COMPLETIONOQ完成This OQ has been completed successfully and is ready for final approval.本OQ已成功完成，有待批准。Signature:签名Date:日期FINAL REVIEW OF DATA AND APPROVAL数据最终审核及批准DEPARTMENT部门PRINT NAME/TIT

2、LE姓名/职务SIGNATURE 签名DATE日期SYSTEM OWNER系统所属部门QA质量保证部APPROVAL DATE:批准日期COMMENTS 备注Purpose: To identify all the individuals who sign or initial any data sheets in this protocol. 目的： 识别所有签字和草签本方案任何数据表的人员。SIGNATURE/INITIALS LOG签名/草签确认PRINT NAME姓名TITLE/COMPAMY职务/公司SIGNATURE签名INITIALS草签TRAINED ON PROTOCOL (

3、Y/N)是否接受方案的培训 （是/否）DATE日期GENERAL REQUIREMENTS要求1) Execution Rules & Practices 执行原则Each test will be performed according to the established testing procedure. If any additional information needs to be documented, the comments section will be used. The acceptance criteria are considered to be met when

4、 the collected data demonstrated that the equipment condition and/or operation are consistent with the requirements and acceptance criteria described in this protocol. The person who executes this protocol will sign their name or initials and date in the COMPLETED BY box. The data obtained will be r

5、eviewed by a second person to certify that the test was performed completely and this person will sign their name or initials and date in the REVIEWED BY box. Good Documentation Practices (KSP SOP QA-011) will be followed during execution of the protocol.依照方案中的测试程序执行每一个测试。在备注栏记录附加信息。若所收集的数据证明设备的状态或运

6、行符合方案中规定的要求及验收标准即可判定符合验收标准。方案执行者在填表人一栏中签名及日期。要求第二个人审核数据以确实执行过程及结果，并在审核人一栏中签名及日期。方案执行中需遵照良好的文件记录规范（KSP SOP QA-011）。2) Exceptional Condition 异常情况When expected results do not meet acceptance criteria or deviation to an approved protocol, an exceptional condition (EC) is triggered. Any EC will lead to a

7、 check mark in “No” box for answering the question of “Acceptance Criteria met?” Record the sequential EC# (01, 02 etc.) on the bottom of the applicable page. Reference and document each deviation on EXCEPTIONAL CONDITIONS SHeET. 未达到预期验收标准或与方案产生偏差将引发异常情况（EC）。若出现任何EC，在回答“是否符合验收标准”时应在“否”选项中打钩。在适当页填写EC

8、序列号（如01，02等）。在异常情况表格中记录每一个异常情况。TABLE OF CONTENTS4. GC Oven Temperature Accuracy and Stability 7 GC柱箱温度的准确度和稳定性 75. Headspace Vent and Pressurization Valve Integrity 9 顶空口和加压阀完整性 96. Headspace Heated Zones Temperature Accuracy 10 顶空加热区温度准确度 107. Inlet Pressure Decay(Channel 1) 11 进样口压力衰减（通道1） 118. In

9、let Pressure Accuracy(Channel 1) 12 进样口压力准确度（通道1） 129. Detector Flow Accuracy(Channel 1) 13 检测器流速准确度（通道1） 1310. Signal Noise and Drift(Channel 1) 15 信号噪音和漂移（通道1） 1511. Signal to Noise(Channel 1) 17 信噪比（通道1） 1712. Injection Precision(Channel 1) 19 进样精密度（通道1） 1913. Inlet Pressure Decay (Channel 2) 20

10、进样口压力衰减（通道2） 2014. Inlet Pressure Accuracy(Channel 2) 21 进样口压力准确度（通道2） 2115. Detector Flow Accuracy(Channel 2) 22 检测器流速准确度（通道2） 2216. Signal Noise and Drift(Channel 2) 24 信号噪音和漂移（通道2） 2417. Signal to Noise(Channel 2) 27 信噪比（通道2） 2718. Injection Precision(Channel 2) 29 进样精密度（通道2） 2919. Injection Carr

11、y Over(Channel 2) 30 进样残留（通道2） 3020. TRAINING VARIFICATION 31培训确认 3121. ATTACHMENT INDEX TABLE 32附件索引表 32SCOPE AND PURPOSE范围和目的The purpose of carrying out OQ is to establish documented evidence that the GC running correctly。本方案是为了建立文件证据来证明QC化学实验室的GC仪器运行正常。RESPONSIBILITY职责Responsibilities of differen

12、t department/personnel involved in different activities related to the OQ of the GC are as follows：与GC运行确认有关的参与不同活动的不同部门/人员的职责如下：2.1 System Owner 系统所属部门The System Owner is responsible for ensuring that GC is in compliance with cGMP. In addition, the System Owner is responsible for the following vali

13、dation-specific tasks:系统所属部门负责确保GC符合cGMP的要求。系统所属部门在验证方面的职责如下： Review and approve OQ protocol and report.审核和批准运行确认方案和报告。 Perform OQ work per protocol, generate report.根据计划开展运行确认工作，完成报告。 Monitor and track all data collected during the OQ study.运行确认期间监控、追踪所有数据。2.2 Quality Assurance (QA) 质量保证Quality Ass

14、urance (QA) is responsible for ensuring that GC and related OQ documentation are in compliance with the cGMP and related KSP procedures. In addition, Quality Assurance is responsible for the following:质量保证部(QA)负责确保GC及相关运行确认文件符合KSP规程。另外，质量保证部的职责如下： Review and approve the OQ documents.审核和批准运行确认文件。SYST

15、EM REFERENCES 系统参考文献Document No.文件编号Approved Y/N批准 是/否1.Agilent 7890 Series GC IOQ Protocol 安捷伦7890系列气相色谱仪IOQ方案IOQ-10-010 Y * REFERENCE AND DOCUMENT ANY DISCREPANCIES ON THe EXCEPTIONAL CONDITIONS SUMMARY在异常情况汇总中引用和记录任何不符合项COMMENTS备注ACCEPTANCE CRITERIA: PRE QUALIFICATION DOCUMENTS FOR THe SYSTEM EXI

16、ST AS REQUIRED.验收标准：确认前，相关文件均已按照要求具备。Acceptance Criteria met?是否符合验收标准？Yes是:No否: If No, Enter EC# _如果为否，输入异常情况编号GC Oven Temperature Accuracy and Stability GC柱箱温度的准确度和稳定性Test Purpose测试目的This test uses a calibrated digital thermometer to determine temperature accuracy and stability.用校验过的数显温度计测定温度的准确度和稳

17、定性。Necessary Instrument必要仪器Digital thermometer数字温度计Preconditions前提Calibration certificate of digital thermometer should be available. 数字温度计具备校验证书。Note 注意In this test, the temperature accuracy is calculated as the absolute difference between the measured temperature and setpoint. The temperature stab

18、ility is calculated as the absolute difference between the highest and lowest measured temperatures.本测试中温度准确度是以测定温度和设定值之间的绝对值来计算。温度稳定性是以最高测定温度和最低测定温度之间的绝对值计算。Test Procedure:测试步骤1Set up the temperature of oven at 230.0C and allow it to stabilize.Use the digital thermometer to measure and record the t

19、emperature.将柱箱的温度设定为230.0C并使之稳定。用数显温度计测量并记录温度。2Set up the temperature of oven at 100.0C and allow it to stabilize.Use the digital thermometer to immediately measure and record the temperature reading, and then measure and record five subsequent temperature readings at intervals of four minutes.将柱箱的温

20、度设定为100.0C并使之稳定。立即用数显温度计测量温度并记下读数。然后每隔至少四分钟测定并记录一次温度读数，记录5次。Measurements and Results:测量结果Procedure步骤Setpoint设定值Measurements测定值Average平均值High最高值Low最低值Accuracy准确度Limit限度Sability稳定性Limit限度1230.0C CN/AN/AN/A C5.0CN/AN/A2100.0C1). C C3.7C1.02). C3). C4). C5). C6). CConclusion:结论： Pass通过 Fail 失败Headspace

21、Vent and Pressurization Valve Integrity 顶空口和加压阀完整性Test Purpose测试目的This tests verifies that the headspaces vent and pressurization valves operate properly. It verifies that there are no excessive leaks and the internal flow paths are not blocked.本测试是为了证明顶空口和加压阀运转正常，没有过度泄露，内部流路没有阻塞。Necessary Instrumen

22、t必要仪器N/A Preconditions前提N/ANote 注意N/A Test Procedure:测试步骤1Connect a 1/8 inch piece of tubing to the vent exit and place the free end of the tube in a beaker of water.将一段1/8英寸的管子连接到顶空口出口处并将另一端置于一个装有水的烧杯中。2Turn off the headspace sampling valve and complete that part of the Results section.关掉顶空采样阀并完成结果

23、章节的相应部分。3Turn on the headspace sampling valve and complete that part of the Results section.打开顶空采样阀并完成结果章节相应部分。Results: 结果：1. Headspace Valve Off 顶空阀门关闭Items项目Observed Result观察到的现象Expected Result期望的结果Conclusion结论a Do bubbles appear as the vial is pressurized?当阀门加压时，是否有气泡出现？Yes有 No没有No没有Pass通过Fail 失败

24、b Does a burst of bubbles appear as the vent valve is opened?当顶空口阀门打开时是否有爆发出气泡？Yes有 No没有Yes有Pass通过Fail 失败c Do bubbles stop after the initial burst?气泡在最初的爆发后是否停止？Yes有 No没有Yes有Pass通过Fail 失败2. Headspace Valve On 顶空阀门开启Items项目Observed Result观察到的现象Expected Result期望的结果Conclusion结论a Do bubbles appear as th

25、e vial is pressurized?当阀门加压时，是否有气泡出现？Yes有 No没有No没有Pass通过Fail 失败b Does a burst of bubbles appear as the vent valve is opened?当顶空口阀门打开时是否有爆发出气泡？Yes有 No没有Yes有Pass通过Fail 失败c Do bubbles stop after the initial burst?气泡在最初的爆发后是否停止？Yes有 No没有Yes有Pass通过Fail 失败Overall Conclusion：总结论： Pass通过 Fail 失败Headspace He

26、ated Zones Temperature Accuracy 顶空加热区温度准确度Test Purpose测试目的This test uses a digital thermometer to determine temperature accuracy of the headspaces heated zones.本测试用数字温度计来检测顶空加热区的温度准确度。Necessary Instrument必要仪器Digital thermometer数字温度计Preconditions前提Calibration certificate of digital thermometer should

27、 be available. 数字温度计具备校验证书。Channel通道2Note 注意In this test, the temperature accuracy is calculated as the absolute difference between the measured temperature and setpoint.本测试中，温度的准确度是以测量温度和设定温度之间的绝对值来计算的。Test Procedure:测试步骤1Set up the oven temperature of headspace heated zones at 100.0C and allow it

28、to stabilize. Use the digital thermometer to measure and record the temperature.将顶空加热炉温度设置为100.0C并使之稳定。用数字温度计测量并记录温度。2Set up the sample loop temperature of headspace heated zones at 110.0C and allow it to stabilize. Use the digital thermometer to measure and record the temperature.将顶空加热区样品循环温度设置为110

29、.0C并使之稳定。用数字温度计测量并记录温度。Measurements and Results:测量结果Procedure步骤Setpoint设定值Measurements测定值Accuracy准确度Limit限度1100.0C C C4.0C2110.0CC C4.0CConclusion:结论： Pass通过 Fail 失败Inlet Pressure Decay(Channel 1) 进样口压力衰减（通道1）Test Purpose测试目的This test demonstrates the pressure integrity of the GC inlet and all flows controlled by the GC inlet pneumatics.本测试是为了证明GC进样口和所有由GC进样口气动装置控制的气流的压力完整性。Necessary In