1. 通则
1. General
Physical tests performed for release purposes need to be validated. The physical test that is comprised in this validation procedure is Particle Size Distribution by Laser Diffraction Instruments.
This SOP can serve as the validation protocol for validating a method for particle size distribution.
A separate validation protocol is necessary in case of an exception from this SOP.
当物理测试作为放行目的的时候应被验证。本验证程序中包含的物理测试是通过激光粒度仪测试样品的粒度分布。该SOP可以作为验证粒度分布方法的协议。若有异议，可以有一个单独的验证方案。
2. 目的
2. purpose
2.1 To define the typical analytical parameters that should be considered when a validation of an analytical method is performed.
2.1 当执行一个分析方法验证的时候，应考虑典型分析参数的定义。
2.2 To describe the way in which a method is validated according to these parameters
2.2 描述按照这些参数进行方法验证的方法。
2.3 To establish acceptance criteria for acceptance / rejection of drug substances, finished products or other materials.
2.3 建立原料药，成品或其它原料的放行/拒绝标准。
3. 范围
3. Range
4. 责任
4. Responsibility
4.1 Physical R&D laboratory analyst – performance of all laboratories studies required for method validation according to this SOP.
4.2 Physical R&D Laboratory manager –
4.2.1 Verification to compliance of this Physical R&D laboratory with GMP regulations and this SOP.
4.2.2 Approval of validation protocol (when applicable) and validation report.
4.3 QC Laboratory manager (only if an interlaboratory study is performed in the QC laboratory):
4.3.1 Verification of compliance of the QC laboratory, with GMP regulations with this SOP and the validation protocol.
4.3.2 To perform the Interlaboratory study.
4.3.3 Approval of validation protocol (when applicable) and validation report.
4.4 QA manager – approval of validation protocol (when applicable) and validation report.
5. 分析参数的定义
DEFINITION OF ANALYTICAL PARAMETERS
In order to prove the analytical capability of a method that assesses physical properties of powder or other solid materials, three main analytical parameters are relevant:
为了证明分析方法的可行性，评估粉末或其它固体原料的物理性质，下面三个主要的分析参数是比较重要的：
Precision
精密度
Accuracy
准确度
Robustness
耐用性
5.1 精密度
5.1  Precision
The precision expresses the closeness of agreement between a series of measurements obtained from multiple sampling of a homogeneous sample.
精密度是指同一样品进行多次取样测试后的一致程度。
The method precision should be assessed in three levels:
方法精密度应评估下列三个方面
Repeatability refers to the use of analytical procedure within a laboratory over a short period of time using the same analyst with the same equipment.
重复性指的是同一分析人员用同一台仪器在间隔很短的时间内使用同一分析方法分析样品。
Intermediate precision (ruggedness) express within laboratory variation, as on different days, or with different analysts or equipment within the same laboratory.
中间精密度是指在同一实验室内，不同天，不同分析人员使用不同仪器分析样品。
Interlaboratory study (reproducibility or technical transfer) refers to the use of the analytical procedure in different laboratories
重现性是指不同实验室之间的研究。
5.2 准确度
5.3 Accuracy
The accuracy of the particle size method is defined as the closeness of test results obtained by the analytical procedure to the true value. Accuracy of sample preparation is achieved when the results includes all the particles as they are presented by an independent method – microscope.
粒度方法的准确度是指通过分析方法测得的粒度值与真实值的接近程度。
5.4 耐用性
5.5 Robustness
The robustness expresses the sensitivity of the method to small, but deliberate variations in the method parameters and provides an indication of its reliability during normal use and stability of the suspension during the measurement.
耐用性是指分析参数故意发生微小变化时分析方法的灵敏度，为正常使用时的重复性和在测试阶段悬浮液的稳定性提供指示。
validation verification6 验证方案
6. Validation protocol
6.1 Any deviation from the SOP should be specified in a validation protocol. If there are no deviations, this SOP can serve as the validation protocol.
6.1 任何偏离本SOP的偏差应在方案中被指出。如果没有偏差，本SOP可以作为验证方案。
6.2 Any major change in the protocol, due to difficulties encountered in the method development work, should be reflected in amendment to the protocol.
6.2 由于在方法开发阶段遭遇的困难，方案中任何主要的变更应反映在方案的修正案中。
7 方法验证的一般程序
7  Generan procedure for validation of a method
Validation of PSD methods is performed on three representative samples.
PSD的方法验证应选取三批样品。
It is possible to perform validation on one or two representative samples in case that additional representative sample/s will not be available, the validation should be completed when additional representative sample/s will be available (as an amendment to validation).