1224方法转移中英文

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〈1224〉TRANSFER OF ANALYTICAL PROCEDURES

INTRODUCTION

Testing to the specification of an ancillary material, intermediate, and/or ingredient and product is critical in establishing the quality of a finished dosage form. The transfer of analytical procedures (TAP), also referred to as method transfer, is the documented process that qualifies a laboratory (the receiving unit) to use an analytical test procedure that originated in another laboratory (the transferring unit), thus ensuring that the receiving unit has the procedural knowledge and ability to perform the transferred analytical procedure as intended.

The purpose of this general information chapter is to summarize the types of transfers that may occur, including the possibility of waiver of any transfer, and to outline the potential components of a transfer protocol. The chapter does not provide statistical methods and does not encompass the transfer of microbiological or biological procedures.

引言

测试，以规范的辅助材料，中间，和/或原料和产品是在建立一个成品剂型质量的关键。分析程序的转移（TAP），也是指方法转移，是一个文件处理程序一个合格的实验室（接收单位）去使用一个分析方法程序源于另一个实验室（转让单位）。确保接受单位有程序性知识和能力去执行方法转移。

这一般信息章节的目的是总结这可能发生的各种转移的类型，包括任何转让的可能性，和概述潜在转移协议组分。本章不提供的统计方法，并不包括转让微生物或生物程序。

TYPES OF TRANSFERS OF ANALYTICAL PROCEDURES

TAP can be performed and demonstrated by several approaches. The most common is comparative testing performed on homogeneous lots of the target material from standard production batches or samples intentionally prepared for the test (e.g., by spiking relevant accurate amounts of known impurities into samples). Other approaches include covalidation（协同验证）between laboratories, the complete or partial validation of the analytical procedures by the receiving unit, and the transfer waiver, which is an appropriately justified omission of the transfer process. The tests that will be transferred, the extent of the transfer activities, and the implementation strategy should be based on a risk analysis that considers the previous experience and knowledge of the receiving unit, the complexity and specifications of the product, and the procedure.

分析程序的转移类型

分析程序的转移可以有几种方法实施及论证。最常见的是同质批次标准生产批号或特意制备的样品测试（例如，样品中加入已知杂质的准确的量）的目标材料进行比较测试。其他方法包括，在实验室之间的验证，由接收单位进行的分析方法的完全的或部分的验证，转移减免，这是一个适当的减少转移程序繁琐的过程。这些测试的变化，转移活性的范围，执行策略将依据风险分析，之前的经验，接收单位的认识，复杂性，产品的规格及程序来进行。

Comparative Testing

Comparative testing requires the analysis of a predetermined number of samples of the same lot by both the sending and the receiving units. Other approaches may be valid, e.g., if the receiving unit meets a predetermined acceptance criterion for the recovery of an impurity in a spiked product. Such analysis is based on a preapproved transfer protocol that stipulates the details of the procedure, the samples that will be used, and the predetermined acceptance criteria, including acceptable variability. Meeting the predetermined acceptance criteria is necessary to assure that the receiving unit is qualified to run the procedure.

比较测试

比较测试要求由转移单位和接收单位分析指定数量的相同样品。其他方法也可有效，例如，如果接收单位预先制定了验收准则可以在产品中包含已知杂质。此分析基于预先批准的转移协议所保证的程序的细节，将用到样品，和预先制定的接收规则，包括可接受的变性。汇总可接受的接受规则是必要地以确保接受单位有资格运行这个程序是有必要的。

Covalidation（协同验证）Between Two or More Laboratories

The laboratory that performs the validation of an analytical procedure is qualified to run the procedure. The transferring unit can involve the receiving unit in an interlaboratory covalidation, including them as a part of the validation team at the transferring unit and thereby obtaining data for the assessment of reproducibility. This assessment is made using a preapproved transfer or validation protocol that provides the details of the procedure, the samples to be used, and the predetermined acceptance

Validation of Compendial Procedures 1225

about which characteristics are appropriate for testing.

两个及以上的实验室的共同验证

实验室完成一个分析程序的确认后即有资格进行此程序。转移单位及接收单位可伴随进行多个实验室验证，他们自己可包含进去作为转移单位验证团队的一部分，从而可获得重复性评价的数据。这个评价由预先转移的或验证协议中程序的细节获得，用到了样品，及预先制定的接收标准。此通则“药典程序的验

证（1225）”中的规定为测试适合的特征提供了有用的指导。

Revalidation（重新验证）

Revalidation or partial revalidation is another acceptable approach for transfer of a validated procedure.

Those characteristics described in 1225, which are anticipated to be affected by the transfer, should be addressed

重新验证.

重新验证或部分重新验证是另一种可接受的验证过程的方法转移。特征描述在章节1225中，预计转移中可能的影响，应该被解决。

Transfer Waiver

The conventional TAP may be omitted under certain circumstances. In such instances, the receiving unit is considered to be qualified to use the analytical test procedures without comparison and generation of interlaboratory comparative data. The following examples give some scenarios that may justify the waiver of TAP:

?Th e new product’s composition is comparable to that of an existing product and/or the concentration of active ingredient is similar to that of an existing product and is analyzed by

procedures with which the receiving unit already has experience.

?The analytical procedure being transferred is described in the USP–NF, and is unchanged.

Verifiction should apply in this case (see 1226).

?The analytical procedure transferred is the same as or very similar to a procedure already in use.

?The personnel in charge of the development, validation, or routine analysis of the product at the transferring unit are moved to the receiving unit.

If eligible for transfer waiver, the receiving receiving unit should document it with appropriate justifications. 转移减免

一般分析方法的转移可能在某种情况下会被忽略。举例说明，接受单位被认为能胜任使用分析使用程序在没有对比试验和多个试验数据比较的情况下。以下几个例子给出了一些可以减免转移分析程序的情况：

●新产品的组分与现有产品和/或现有产品的主要活性成分的浓度相似，并且接收单位对现有产品已经有

成熟分析程序。

●转移的分析程序在USP–NF中被描述，且没有改变。这样情况下适用于确认（见1226）。

●转移分析程序与已经使用的程序相同或非常相似。

转移单位负责产品发展，验证，或常规分析的人员去了接收单位。

如果条件符合转移减免，接受单位应当取证证明。

ELEMENTS RECOMMENDED FOR THE TRANSFER OF ANA YTICAL PROCEDURES

所推荐的分析方法转移的原理

Several elements, many of which may be interrelated, are recommended for a successful TAP. When appropriate and as a part of pretransfer activities, the transferring unit should provide training to the receiving unit, or the receiving unit should run the procedures and identify any issues that may need to be resolved before the transfer protocol is signed. Training should be documented.

一些相关的原理，许多是成功的分析方法转移所推荐的。当适当的和作为预先转移活性的一部分，转移单位应对接收单位提供培训，或接收单位应运行此程序并且在签订转移协议之前将所有问题解决。培训应当被记录。

The transferring unit, often the development unit, is responsible for providing the analytical procedure, the reference standards, the validation reports, and any necessary documents, as well as for providing the necessary training and assistance to the receiving unit as needed during the transfer. The receiving unit may be a quality control unit, another intracompany facility, or another company such as a contract research organization. The receiving unit provides qualified staff or properly trains the staff before the transfer, ensures that the facilities and instrumentation are properly calibrated and qualified as needed, and verifies that the laboratory systems are in compliance with applicable regulations and in-house general laboratory procedures. Both the transferring and receiving units should compare and discuss data as well as any deviations from the protocol. This discussion addresses any necessary corrections or updates to the final report and the analytical procedure as necessary to reproduce the procedure.

转移单位，经常是开发单位，在转移过程中负责提供分析程序，参考标准，验证报告，及其他必要的证明，同时根据接受单位的需要提供必要的培训及援助。接收单位可能是一个质量控制单位，或另一个公司内部的部门，或另一个公司如一个研究机构。在转移前接收单位提供有资质的人员或适合接受培训的人员，确保设备及使用仪器经过适当的校准并具备需要的资质，并核实实验室系统按照合适的规程和厂内一般的实验室规程。转移及接收单位应对比并讨论任何与协议出现偏差的数据。将讨论的任何修正或更新到补充到最终报告和分析程序是有必要的。

A single lot of the article may be used for the transfer, because the aim of the transfer is not related to the manufacturing process but rather to the evaluation of the analytical procedure’s performance at the receiving site.

在许多文章中单一的一点都可能被用于转移，因为转移旨在是不涉及到制造业的程序，而是分析程序在现场执行的评估。

PREAPPROVED PROTOCOL预先批准的协议

A well-designed protocol should be discussed, agreed upon, and documented before the implementation of TAP. The document expresses a consensus between the parties, indicating an intended execution strategy, a nd should include each party’s requirements and responsibilities. It is recommended that the protocol contain the following topics as appropriate: objective, scope, responsibilities of the transferring and receiving units, materials and instruments that will be used, analytical procedure, experimental design, and acceptance criteria for all tests and/or methods included in the transfer. Based on the validation data and procedural knowledge, the transfer protocol should identify the specific analytical performance characteristics (see 1225and1226) that will be evaluated and the analysis that will be used to evaluate acceptable outcomes of the transfer exercise.

一个设计好的协议在分析方法转移之前应该经过讨论，同意和证明的。该文件表示在各方之间达成共识，表明预期的执行策略，并应包括每一个方面的要求和责任。被推荐的协议视情况包含以下几点：转移及接收单位的目的，范围，职责，将用到的材料和设备，分析过程，实验设计，和所有要转移的试验和/或方法接受标准。基于验证数据和过程知识，转移协议应鉴定专属性（见1225和1226），它将被评估和分析，将用于评估转移行为可接受的效果。

The transfer acceptance criteria, which are based on method performance and historical data from stability and release results, if available, should include the comparability criteria for results from all study sites. These criteria may be derived using statistical principles based on the difference between mean values and established ranges and should be accompanied by an estimation of the variability (e.g., percent relative standard deviation [%RSD] for each site), particularly for the intermediate precision %RSD of the receiving unit and/or a statistical method for the comparison of the means for assay and content uniformity tests. In instances of impurity testing, where precision may be poorer such as in the case of trace impurities, a simple descriptive approach can be used. Dissolution can be evaluated by a comparison of the dissolution profiles using the similarity factor f2 or by comparison of data at the specified time points. The laboratories should provide appropriate rationale for any analytical performance characteristic not included. The materials, reference standards, samples, instruments, and instrumental parameters that will be used should be described.

转移接受的标准，基于方法的实施和来自稳定性测定的历史数据和发行的结果，如果可用，应当包括所有研究地点的结果的可比较性标准。这些标准可能得自于由统计学原理计算的基于平均值之间的差异和建立范围，并应伴随着变异的评估（如来自于每个站点的相对标准偏差的，{%RSD}）特别是接收单位和/或统计方法为手段的比较测定和含量一致性测试的中间精密度的相对标准偏差的百分比，和化验方法的比较的统计学分析。举例说明杂质的测试，在痕量杂质的测试中精密度非常难掌握，可以用一个简单的描述方法。可以溶解的溶出度比较相似因子f2或在指定的时间点的数据进行比较评估。实验室应为分析特性提供适用的原理。应该描述所用到的材料，参考标准，样品，仪器，仪器参数。

It is recommended that expired, aged, or spiked samples be carefully chosen and evaluated to identify potential problems related to differences in sample preparation equipment and to evaluate the impact of potential aberrant results on marketed products. The documentation section of the transfer protocol may include report forms to ensure consistent recording of results and to improve consistency between laboratories. This section should contain the additional information that will be included with the results, such as example chromatograms and spectra, along with additional information in case of a deviation. The protocol should also explain how any deviation from the acceptance criteria will be managed. Any changes to the transfer protocol following failure of an acceptance criterion must be approved before collection of additional data.

推荐慎重选择过期，成熟或加标样品去鉴别潜在的问题关于不同的样品准备和评估销售的产品潜在的异常结果的影响。转移协议文件的部分章节可能包含报告形式来确保对结果记录的一致性，并提高实验室之间的一致性。这部分应包含带有结果的附加信息，如色谱图和光谱图，以及偏差情况下的额外信息。协议应说明任何验收标准的偏差应管理。转移协议任何的变化跟随着接受标准的失败，在附加数据确认之前要被核实。

THE ANALYTICAL PROCEDURE 分析程序

The procedure should be written with sufficient detail and explicit instructions, so that a trained analyst can perform it without difficulty. A pretransfer meeting between the transferring and receiving units is helpful to clarify any issues and answer any questions regarding the transfer process. If complete or partial validation data exist, they should be available to the receiving unit, along with any technical details required to perform the test in question. In some cases it may be useful for the individuals who were involved with the initial development or validation to be on site during the transfer. The number of replicates and injection sequences in the case of liquid or gas chromatography should be clearly expressed, and, in the case of dissolution testing, the number of individual dosage units should be stipulated.

程序被记录时要有充分的细节描述，及清楚地指示，以便完成分析者培训时没有困难。在转移单位与接收单位之间的预先转移会议对阐明问题，答案是有帮助的。如果全部或部分验证数据的存在，他们应该提供给

接收单位，以及执行中的问题的测试所需的任何技术细节。在一些事件中，它可能对一些初步发展和进行实地验证的人是有用处的在转移期间。应清楚描述液相或气相进针次数和进针序列，在溶出度测量中，单一的剂量应被规定。

TRANSFER REPORT 转移报告 When the TAP is successfully completed, the receiving unit should prepare a transfer report that describes the results obtained in relation to the acceptance criteria, along with conclusions that confirm that the receiving unit is now qualified to run the procedure. Any deviations should be thoroughly documented and justified. If the acceptance criteria are met, the TAP is successful and the receiving unit is qualified to run the procedure. Otherwise, the procedure cannot be considered transferred until effective remedial steps are adopted in order to meet the acceptance criteria. An investigation may provide guidance about the nature and extent of the remedial steps, which may vary from further training and clarification to more complex approaches, depending on the particular https://www.360docs.net/doc/5011050019.html,P35 当TAP 成功完成后，接收单位应准备转移报告，介绍取得有关验收标准，结果和结论，确认接收单位有资格运行程序。任何的偏差都应该记录并详细说明。如果接受标准通过，分析方法的转移即为成功，接收单位可进行此程序。否则，此程序不能被转移，直到采用有效的补救措施来适合接受标准。调查可能会提供有关补救措施的性质和补救步骤的程度，进一步培训和澄清，以更复杂的方法可能会有所不同，具体取决于特定程序

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