发布时间 : 星期二 文章中英对照-APIC 原料药厂清洁验证指南：8.0残留量检测更新完毕开始阅读
本章列出了根据清洁程序中最后一次淋洗液中残留量，计算清洁后设备中残留量的定量方法。
The residue amount in the equipment can be assumed to be equal to the amount of residue in the last wash or rinse solvent portion. The assumption is based on the worst case consideration that a further rinse (or any reaction) would not remove more than the same amount of residue present in the analysed rinse sample.
可以假定设备中残留量等于最后冲洗或淋洗溶剂中的总量。该假设是基于最差情形考虑，即进一步淋洗（或任何反应）将无法得到比分析用淋洗样品结果更高的残留物。
The advantage of the rinse sampling method is the whole equipment will be reached by the solvent, including difficult to reach locations that cannot be disassembled. Therefore, if appropriately designed, this method will give the best indication of the amount of residue remaining in the equipment.
淋洗取样方法的优点是整个设备都会被溶剂洗到，包括最难触及且不能拆卸的部位。因此，如果对淋洗方法进行了适当的设计，该方法能最好地显示设备中残留量。
For quantitation, a solvent sample (e.g. 1 litre) is removed and the residue in the sample is determined by a suitable analytical method, which can then be extrapolated to the whole equipment according to Equation 5. 在定量检测时，取一个溶剂的样品（例如1L），对样品中的残留采用适当的分析方法进行检测，然后根据公式5外推至整个设备。 Equation 5: M = V × (C – CB) Where 其中 M Amount of residue in the cleaned equipment in mg. 清洁后的设备中的残留量mg Volume of the last rinse or wash solvent portion in litres. 最后淋洗或冲洗溶剂体积， Concentration of impurities in the sample in mg/l. 样品中杂质浓度，mg/l CBBlank of the cleaning or rinsing solvent in mg/l. If several samples are taken during one run, one and the same blank can be used for all samples provided the same solvent lot was used for the whole run.清洁或淋洗溶剂空白水平，mg/l如果在一个轮次中取了几个样品，并且在整个轮次中使用的溶剂是同一个批号，则可以在所有样品计算中使用同一个空白。8.3.3 Stamps 邮戳法
In this exceptionally used sampling method, “coins” (or stamps) are placed on appropriate sampling points in the equipment during the manufacture of the previous product and during cleaning. After cleaning, the contamination on the coins can be analysed and the overall contamination can be calculated by extrapolation to the whole equipment. For quantitation, the coins may be firstly swabbed followed by further analysis of the samples.
这是一种在例外情况下使用的取样方法。取一个“圆片”（或邮票），置于设备中适当的取样点上，进行上一产品的生产及清洁。在清洁后，对硬币上的污染物进行检测，采用外推法计算整个设备的全部污染。如果是要进行定量分析，则对圆片进行擦拭取样，然后对样品进行进一步分析。 8.4 Analytical Methods 分析方法
A sample isolated by either of the sampling methods discussed in Section 8.3 should be analysed by a suitable analytical method (e.g. HPLC, GC, GC-MS, TLC, dry residue, TOC, UV, titration, conductivity or pH). The suitability of the method can be documented by appropriate validation as detailed in Section 8.2.
按第8.3部分所讨论的取样方法之一所获得的样品应采用适当的分析方法（例如，HPLC、GC、GC-MS、TLC、蒸发残渣、TOC、UV、滴定、电导率或pH值）进行检测。方法的适用性可以依据8.2部分指导进行适当的验证并记录。
A combination of analytical methods can be used if appropriate. For example evaporation of the solvent sample and analysis of the dry residue by another method (e.g. HPLC) can enhance the sensitivity of the final analytical method by a factor 106. Alternatively, the use of several methods (e.g. titration, HPLC) can provide the required specificity. 适当时，可以合并使用几个分析方法。例如，将溶剂样品蒸发，采用另一个方法（例如HPLC）分析残渣。这样可以增加最后分析方法的灵敏度到100万倍；而采用几个方法（例如，滴定、HPLC）可以达到所需的专属性。