[技术帖] 美国药典委员会微信问答合集

制药圈

2015年2月问题:

《美国药典-国家处方集》(USP-NF)中的通用检测方法收录在通则(General Chapter)中,所有的通则都是强制执行的吗?

回答:

在USP37-NF32 第二增补本的凡例(General Notice)中“2.OFFICIAL STATUS AND LEGAL RECOGNITION”项下有如下规定:

“2.10. Official Text

Official text is text contained in USP and NF, including monographs, general chapters, and these General Notices. Revisions to official text are provided in supplements, Interim Revision Announcements, and Revision Bulletins. General chapters numbered from 1000 to 1999 are considered interpretive and are intended to provide information on, give definition to, or describe a particular subject. They contain no mandatory requirements applicable to any official article unless specifically referenced in General Notices, a monograph, or a general chapter numbered below 1000. General chapters numbered above 2000 apply only to articles that are intended for use as dietary ingredients and dietary supplements.”


2015年3月问题:

在"炽灼残渣 (Residue on Ignition)"和"干燥失重 (Loss on Drying)"测试中,会有要求"恒重(Constant Weight)",根据《美国药典-国家处方集》(USP-NF)的规定:"恒重"表示样品连续两次炽灼或干燥后称重的差异不得超过多少重量呢?

回答:

在USP37-NF32 第二增补本的凡例(General Notice)中“6. TESTING PRACTICES AND  PROCEDURES”项下有如下规定:

6.40.10. Ignite to Constant Weight "Ignite to constant weight” means that ignition shall be continued at 800 ± 25, unless otherwise indicated, until two consecutive weighings, the second of which is taken after an additional period appropriate to the nature and quantity of the residue, do not differ by more than 0.50 mg per g of substance taken.


6.40.20. Dried to Constant Weight "Dried to constant weight” means that drying shall be continued until two consecutive weighings, the second of which is taken after an additional drying period appropriate to the nature and quantity of the residue, do not differ by more than 0.50 mg per g of substance taken.


2015年4月问题:

USP会对药典测试即将不再有效的前一批次(Previous Lot)标准品赋予有效使用日期(Valid Use Date)。问题1:通过什么途径可以查询到先前批次(Previous Lot)USP标准品的有效使用日期?问题2: 若某批次USP标准品标明“Valid Use Date:11/12”,即表示此批次标准品有效使用日期是截止到哪一天呢?

回答:

问题1答案:(1)登录USP官方网站www.usp.org,输入搜索标准品(英文名)或Catalog No.,例如搜索"Sucrose"或其Catalog No.:1623637,即可查询到如下信息:


(2)登录USP官方网站www.usp.org,在"Reference Standards"项下下载“USP Daily Reference Standards Catalog"

(3)订阅USP Email Notice,定期接收来自USP的邮件通知

(4)关注USP官方微信和微博,每月了解USP标准品更新


问题2答案:"Valid Use Date:MM/YY"中,MM表示"月",YY表示"年",有效期为截止至该年该月的最后一天。所以,若某批次USP标准品标明“Valid Use Date:11/12”,即表示此批次标准品有效使用日期是截止到2012年11月30日。


2015年5月问题:

在依据USP各论及相关通则进行色谱法测试时,样品溶液中某组分的相对保留时间必须与各论规定的相对保留时间完全一致吗?为什么?

回答:

在通则<621>色谱法的系统适用性(SYSTEM SUITABILITY)项下有如下描述:

"Relative retention times may be provided in monographs for informational purposes only to aid in peak identification.There are no acceptance criteria applied to relative retention times."

即各论中提及的相对保留时间仅供参考,旨在辅助识别色谱峰,并没有关于相对保留时间的可接受标准"。


2015年6月问题:

USP对贮存条件的描述中,“Cold”是指温度在2℃~8℃之间。这种说法是正确的吗?

回答:

此说法是错误的。在USP38-NF33的通则<659>包装和贮存要求(PACKAGING AND STORAGE REQUIREMENTS) “STORAGE CONDITIONS”项下有如下描述:

"Cold: Any temperature not exceeding 8(46 F)."


特别提醒:

很多朋友在回答时提到"根据USP凡例10中的规定。。。",小编在此特别提醒,事实上,最新生效的USP38-NF33 已对此章节修订: 除非各论有其他要求,凡例10.10中关于包装和贮存要求的内容均已"搬家"至通则<659>PACKAGING AND STORAGE REQUIREMENTS。小编在此特别提醒,并建议大家参考最新生效的药典内容。


2015年7月问题:

在执行USP-NF方法时,若需做红外鉴别,需用样品的红外图谱与USP的红外标准图谱集进行比较,这种说法正确吗?

回答:

此说法是错误的。根据通则“<197> SPECTROPHOTOMETRIC IDENTIFICATION TESTS”规定:

"Record the spectra of the test specimen and the corresponding USP Reference Standard over the range from about 2.6 µm to 15 µm (3800 cm–1 to 650 cm–1) unless otherwise specified in the individual monograph.The IR absorption spectrum of the preparation of the test specimen, previously dried under conditions specified for the corresponding Reference Standard unless otherwise specified, or unless the Reference Standard is to be used without drying, exhibits maxima only at the same wavelengths as that of a similar preparation of the corresponding USP Reference Standard......"

另外,在通则"<851> SPECTROPHOTOMETRY AND LIGHT-SCATTERING"中对于USP标准品用于药典分光光度法测试也有相应规定和描述。

2015年8月问题:

想了解美国药典中对某品种的性状、气味和溶解性的描述,但在该品种各论中却找不到,说明USP-NF未收录产品性状,气味和溶解性的信息。这种说法是正确的吗?

回答:

此说法是错误的。除各论有其他规定外,“Description and Solubility”信息均收载于“Reference Table”项下,且此信息仅作为物质特性初步评估的辅助参考,而非药典标准和纯度测试要求。原文如下:

"The “description” and “solubility” statements pertaining to an  article (formerly included in the individual monograph) are general in nature.  The information is provided for those who use, prepare, and dispense drugs,  solely to indicate descriptive and solubility properties of an article complying  with monograph standards. The properties are not in themselves standards or  tests for purity even though they may indirectly assist in the preliminary  evaluation of the integrity of an article....."

另外,在USP38-NF33 第一增补本的凡例(General Notices: 5. MONOGRAPH COMPONENTS)中“5.30 Description and Solubility” 项下也有详细说明。


2015年9月问题:

USP药典论坛(Pharmacopeia Forum)上提议修订的内容都会按计划收录于《美国药典-国家处方集》吗?如果不是,在哪里可以了解这些修订的进展和状态呢?

回答:

USP药典论坛上提议修订的内容不都会按计划收录于《美国药典-国家处方集》中,有关修订的进展和状态可在USP官方网站查询:登录www.usp.org→USP-NF→Official Test→Proposal status and commentary


2015年10月问题:

USP通则<467>列出了残留溶剂的分类和限度,这些限度是针对制剂产品而非原料、辅料设定的。这个说法是正确的吗?

回答:

此说法是正确的。USP通则<467>列出的残留溶剂限度是针对制剂产品而非原料、辅料设定的。


2015年11月问题:

药典论坛 (Pharmacopeial Forum,PF)是 USP 标准修订的公共平台,它是一个免费网络双月刊,发布后有 90天的公众评议期,它的内容是法定生效文件,用户可直接将其等同于USP-NF使用,这个说法是正确的吗?

回答:

此说法是不正确的。 药典论坛 (Pharmacopeial Forum,PF)是 USP 标准修订的公共平台,它是一个免费网络双月刊,USP在药典论坛 (Pharmacopeial Forum,PF)上发布关于《美国药典-国家处方集》(USP-NF)中的标准修订提案,供公众评议,发布后有 90天的公众评议期,通过PF,用户可以回顾和追踪提议修订的进程并提交修订意见。修订提案并非法定生效文件,不可等同于USP-NF使用。

药典论坛:www.usppf.com


2015年12月问题:

USP提供了药典方法中使用的HPLC和GC色谱柱品牌参数等信息供用户参考,这个说法是正确的吗?

回答:

此说法是正确的。USP-NF方法开发中用到的色谱柱品牌信息收录于免费在线版www.uspchromcolumns.com网站中,注册后即可登录。该数据库可节省用户寻找适用于测试的色谱柱的宝贵时间,追踪从修订阶段到生效状态的方法中使用的色谱柱,查找色谱柱品牌和生产商,找到可使用的备选(或替代)色谱柱等。注:色谱柱品牌名称仅为便于用户参考信息,不包含任何暗示,批准,认可或认证。

色谱柱在线数据库:www.uspchromcolumns.com


2016年1月问题:

根据USP-NF的要求,制剂产品的生产不一定要使用符合USP-NF标准的原辅料,即使USP-NF中收录了该原辅料的标准,这个说法正确吗?

回答:

此说法是错误的。在USP38-NF33第二增补本的凡例3. CONFORMANCE TO STANDARDS中有如下规定:“Official products are prepared according to recognized principles of  good manufacturing practice and from ingredients that meet USP or NF standards, where standards for such ingredients exist (for dietary supplements,  see section 3.10.20).”


2016年2月问题:

USP-NF中的"about"通常是指称量,体积,保留时间的正负偏差值为5%,这个说法正确吗?

回答:

此说法是错误的。在USP38-NF33第二增补本的凡例8. TERMS AND DEFINITIONS中有如下规定:““About” indicates a quantity within 10%.”


2016年3月问题:

当USP标准品标签上明确要求标准品在使用前进行干燥时,为便于操作,通常USP建议用户直接使用原始包装容器对标准品进行干燥,这个说法正确吗?

回答:

此说法是错误的。在USP38-NF33第二增补本的通则<11>USP REFERENCE STANDARDS中对“Dry Before Use”有如下规定:“Use immediately after drying under stated conditions. Drying should not be  performed in the original container. A portion of the material should be  transferred to a separate drying vessel.”


2016年4月问题:

如果有药典方法提供,用户不可使用自己开发的方法替代药典方法,这个说法正确吗?

回答:

此说法是错误的。在USP38-NF33第二增补本的凡例6.30 Alternative and Harmonized Methods and Procedures有如下描述:“Alternative methods and/or procedures may be used if they provide advantages in  terms of accuracy, sensitivity, precision, selectivity, or adaptability to  automation or computerized data reduction, or in other special circumstances.  Such alternative procedures and methods shall be validated as described in the  general chapter Validation of Compendial Procedures 1225 and must be shown to give equivalent or better  results. Only those results obtained by the methods and procedures given in the  compendium are conclusive..”


2016年5月问题:

USP标准品是经 USP 全面标定的高纯度物质,用户购买后可按各种需要使用,这个说法正确吗?

回答:

此说法是错误的。在USP39-NF34的通则<11>USP
REFERENCE STANDARDS中有如下描述:“Reference
Standards for official articles in USP or NF are provided as pure materials or as mixtures of chemicals reflective of the corresponding drug substances or excipients. The use of these materials is specified in the article's monograph, and these materials generally are necessary for use in the Assay and/or the Identification tests. The suitability of a USP RS for uses outside those specified in a monograph is the responsibility of the user."


另外,USP 标准品的Certificate中有如下说明:

Instructions for Use: Follow the instructions in the appropriate USP or NF Monographs and General Requirements for Tests and Assays of the current USP–NF. In the event that instructions on the label of this lot differ from those found in the current USP–NF, those on the label supersede any instructions listed in Chapter <11>.


2016年6月问题:

在USP-NF关于贮存条件的描述中,“Freezer”是指贮存在温度为−25°至−10°的条件下,而"Refrigerator”是指贮存在温度为2°至 8°的条件下,这个说法正确吗?

回答:

此说法是正确的。在USP39-NF34的通则General Chapters<659> PACKAGING AND STORAGE REQUIREMENTS的“STORAGE CONDITIONS”项下有如下描述:

"Freezer: A place in which the temperature is maintained between −25° and −10° (−13° and 14 °F).

Refrigerator: A cold place in which the temperature is maintained between 2° and 8° (36° and 46 °F)."


2016年7月问题:

如果各论中有机杂质检查项下存在多个测试内容(Procedures),那必须完成每个测试内容并符合其接受标准,这个说法正确吗?

回答:

此说法是错误的。在凡例(General Notice) 4.10.10. Applicability of Test Procedures中有如下说明:

A single monograph may include more than one test, procedure, and/or acceptance criterion for the same attribute. Unless otherwise specified in the monograph, all tests are requirements. In some cases, monograph instructions allow the selection of tests that reflect attributes of different manufacturers' articles, such as different polymorphic forms, impurities, hydrates, and dissolution. Monograph instructions indicate the tests, procedures, and/or acceptance criteria to be used and the required labeling.

The order in which the tests are listed in the monograph is based on the order in which they are approved by the relevant Expert Committee for inclusion in the monograph. Test 1 is not necessarily the test for the innovator or for the reference product. Depending on monograph instructions, a labeling statement is not typically required if Test 1 is used.

        

来源:美药典USP。

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