留样观察，只观察成品留样吗，每年观察几批？

safsaf

2010版GMP规定成品的留样：4.如果不影响留样的包装完整性，保存期间内至少应当每年对留样进行一次目检观察，如有异常，应当进行彻底调查并采取相应的处理措施；5.留样观察应当有记录。请问，①留样观察只观察成品留样吗，中间体、起始物料的留样需要观察吗？②成品中的原料药留样每年观察几批，成品中的外销中间体每年观察几批，中间体、起始物料的留样每年观察几批？

lxlltt0214

观察成品的话，每一批次都需要观察。也是给企业做好保护，在产品储存条件下放置是否有可能产生外观性状的改变。

pussay11

原辅料也有留样，仅作备查；中间体在投向的产品生产完成后也销毁了；成品留样每年目检观察，如有异常则进行彻底调查并采取相应的处理措施。原来的厂是这么做的。

幸福萍萍

成品每批都需要留样观察。

beiwei5du

1、各国的法规仅针对于成品进行留样观察，同时ICH q7却没有针对于API留样观察的规定，但是最好进行留样观察；
2、中间体和起始物料是否留样在各国法规上均未有强行规定；
3、关于制剂成品的留样观察，在美国CGMP中有提及，从这个要求中，并不要求每批进行留样观察，但是基于怎样的acceptable statistical procedures需要考虑？？？（根号N+1???）

Except for those for drug products described in paragraph (b)(2) of this section, reserve samples from representative sample lots or batches selected by acceptable statistical procedures shall be examined visually at least once a year for evidence of deterioration unless visual examination would affect the integrity of the reserve sample. Any evidence of reserve sample deterioration shall be investigated in accordance with §211.192. The results of the examination shall be recorded and maintained with other stability data on the drug product. Reserve samples of compressed medical gases need not be retained. The retention time is as follows:

(1) For a drug product other than those described in paragraphs (b) (2) and (3) of this section, the reserve sample shall be retained for 1 year after the expiration date of the drug product.

(2) For a radioactive drug product, except for nonradioactive reagent kits, the reserve sample shall be retained for:

(i) Three months after the expiration date of the drug product if the expiration dating period of the drug product is 30 days or less; or

(ii) Six months after the expiration date of the drug product if the expiration dating period of the drug product is more than 30 days.

(3) For an OTC drug product that is exempt for bearing an expiration date under §211.137, the reserve sample must be retained for 3 years after the lot or batch of drug product is distributed.

beiwei5du

pussay11 发表于 2017-6-29 08:55
原辅料也有留样，仅作备查；中间体在投向的产品生产完成后也销毁了；成品留样每年目检观察，如有异常则进行 ...

但是在美国针对于辅料的留样却没有硬性要求：
411.  Several comments recommended that hazardous and unstable materials be exempt from the reserve sample requirement in 211.170(a).  Other comments suggested that inactive ingredients also be exempted.     The Commissioner has concluded that storage of some types of materials may constitute an unnecessary burden or a safety problem. The section, as revised, will eliminate retention of inactive ingredients.  He believes that deletion of retention requirements for inactive ingredients will eliminate most of the objections regarding hazardous and unstable materials; most of those materials cited by respondents are used as inactive ingredients.  For those active ingredients that may be hazardous, though, the Commissioner concludes that the need for retaining samples of such active ingredients outweighs potential problems of storage.

beiwei5du

lxlltt0214 发表于 2017-6-29 08:53
观察成品的话，每一批次都需要观察。也是给企业做好保护，在产品储存条件下放置是否有可能产生外观性状的改 ...

每批硬性的留样观察时出自于哪里呢？？？

1761696964

beiwei5du 发表于 2017-8-7 14:00
1、各国的法规仅针对于成品进行留样观察，同时ICH q7却没有针对于API留样观察的规定，但是最好进行留样观察 ...

老师，那这个留样观察可以开根号进行目检吗？

biubiuo8r

lxlltt0214 发表于 2017-6-29 08:53
观察成品的话，每一批次都需要观察。也是给企业做好保护，在产品储存条件下放置是否有可能产生外观性状的改 ...

留样观察有标准吗，需要观察些啥