美国药典621

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美国药典标准

猪八戒照镜子歇后语
猪八戒照镜子歇后语
小编相信一提起猪八戒，没有人是不知道的，这是《西游记》贡献给我国文化长廊中的一个经典角色。

虽说那么的好吃懒做。

但也憨厚惹人爱。

民间就流传着很多关于猪八戒的歇后语，可见他的魅力哦：
猪八戒照镜子——里外不是人
【关于猪八戒的歇后语集锦】
猪八戒照镜子——里外不是人
猪八戒的后脊梁——无能之辈（悟能之背）
猪八戒戴花——自美
和尚打伞——无法无天
猪八戒读书——竟冲识字的
八戒保媒把把成功——猪连必合（珠联壁合）
猪八戒进女儿国——看花了眼
猪八戒娶媳妇——背着走
猪八戒背媳妇——舍得花力气
猪八戒不成仙——坏在嘴上
猪八戒吃黄连/猪八戒吃人参果——苦了大嘴的
猪八戒吃猪啼——自残骨肉
猪八戒充英雄——只是嘴皮子拱得欢
猪八戒戴耳环——自以为美
猪八戒戴花——越多越丑
猪八戒的武艺/猪八戒过火焰山/猪八戒耍把式——倒打一耙
猪八戒的嘴巴——自我欣赏
猪八戒掉进万花筒——丑态百出
猪八戒发眸气——又丑又恶
猪八戒拱帘子——嘴先进
猪八戒进了女儿国——看花了眼
猪八戒进屠场——自己贡献自己
猪八戒啃地梨——什么仙人吃什么果
猪八戒了天拜佛——掸心不稳
猪八戒买猪肝——难得心肠
猪八戒卖炒肝——这是哪道肺
猪八戒卖凉粉——样数不多，滋味不少
猪八戒三十六变——没有一副好嘴脸
猪八戒摔镜子——怕露丑
猪八戒西天取经——三心二意
猪八戒相亲——怕露嘴脸
猪八戒想娶媳妇——一厢情愿
猪八戒背媳妇——心甘情愿
猪八戒招亲——黑灯黑人
猪八戒照镜子/猪八戒照像——自找难堪（看）。

聚乙烯吡咯烷酮

聚乙烯吡咯烷酮聚烷酮本专著内容中属于美国药典正文但不属于协调正文的部分已用（）符号标记出。

（C6H9NO）n2-吡咯烷酮，1-乙烯基-，均聚物1-乙烯基-2-吡咯烷酮聚合物9003-39-8定义聚乙烯吡咯烷酮：实际上是由线型1-乙烯-2-吡咯烷酮组成的合成型聚合物，聚合度不同导致聚合物分子量不同。

K值是与聚乙烯吡咯烷酮的水溶液的相对粘度有关的特征值，该参数可表示不同规格的聚乙烯吡咯烷酮。

具有标示K值为15或更低的聚乙烯吡咯烷酮的K值为标示值的85.0%-115.0%。

具有标示K值或K值范围平均值高于15的聚乙烯吡咯烷酮的K值为标示值或标示范围平均值的90.0%-108.0%。

聚乙烯基吡咯烷酮包含不低于11.5%，不高于12.8%的氮（14.01）（以无水物计算）。

其标示K值不低于10不高于120。

标签上显示标示K 值。

鉴定A样品溶液：聚乙烯吡咯烷酮溶液20mg/ml分析：向10ml样品溶液中加入20ml 1mol/l盐酸和5ml重铬酸钾试液验收准则：生成橘黄色沉淀B溶液A：溶解75mg硝酸钴和300mg硫氰酸铵于2ml水中样品溶液：聚乙烯吡咯烷酮溶液20mg/ml分析：混合溶液A和5ml样品溶液，向该溶液中加3mol/l盐酸溶液使其呈酸性验收准则：淡蓝色沉淀生成C样品溶液：聚乙烯吡咯烷酮溶液5mg/ml分析：向5ml样品溶液中加入几滴碘试液验收准则：溶液变为深红色D样品溶液：聚乙烯吡咯烷酮水溶液50mg/ml验收准则：完全溶解化验氮测定方法Ⅱ（461）样品：0.1g聚乙烯吡咯烷酮分析：该过程中忽略双氧水的使用，用硫酸钾，硫酸铜，二氧化钛（33:1:1）的粉状混合物代替硫酸钾，硫酸铜（10:1）。

加热混合物直到得到一个澄清，浅绿色溶液。

继续加热45min，并按指示的程序操作，从“向消化混合物小心加入70ml水”开始。

验收准则：无水物含氮量11.5%-12.8%杂质炽灼残渣（281）不高于0.1%铅（251）测试准备：1.0g溶于25ml水验收准则：不高于10ppm醛限度溶液A：500ml容量瓶中加入8.3g焦磷酸钾，加400ml水溶解。

药典检测项目汇总

项目/参数检测标准（方法）名称及编号（含年号）限制范围序号名称1 一般鉴别反应中国药典2005版一部附录Ⅳ、二部附录II 美国药典第31版<191> 英国药典2007版附录IIB欧洲药典第5版2.2.252 紫外分光光度法中国药典2005版一部附录ⅤA、二部附录ⅣA美国药典第31版<197>英国药典2007版附录II B欧洲药典第5版2.2.253 红外分光光度法中国药典2005版一部附录ⅤC、二部附录ⅣC美国药典第31版<197>英国药典2007版附录II A欧洲药典第5版2.2.244 原子吸收分光光度法美国药典第31版<851>5 薄层色谱法中国药典2005版一部附录Ⅵ B、二部附录ⅤB美国药典第31版<621> 英国药典2007版附录ⅢA欧洲药典第5版2.2.276 高效液相色谱法中国药典2005版一部附录ⅥD、二部附录ⅤD美国药典第31版<621> 英国药典2007版附录Ⅲ D欧洲药典第5版2.2.297 气相色谱法中国药典2005版一部附录Ⅵ E、二部附录Ⅴ E美国药典第31版<621>英国药典2007版附录Ⅲ B欧洲药典第5版2.2.288 熔点测定法美国药典第31版<741> 英国药典2007版附录Ⅴ A 欧洲药典第5版2.2.14-169 旋光度测定法中国药典2005版一部附录Ⅶ E、二部附录Ⅵ E美国药典第31版<781>英国药典2007版附录ⅤF 欧洲药典第5版2.2.710 折光率测定法美国药典第31版<831>英国药典2007版附录ⅤE 欧洲药典第5版2.2.611 黏度测定法中国药典2005版二部附录Ⅵ G美国药典第31版<911>英国药典2007版附录Ⅴ H欧洲药典第5版2.2.9-10不做中国药典第一法12 pH值测定法中国药典2005版二部附录Ⅵ G 美国药典第31版<911>英国药典2007版附录Ⅴ H欧洲药典第5版2.2.9-1013 氧瓶燃烧法中国药典2005版一部附录Ⅷ A、二部附录Ⅶ A美国药典第31版<541>英国药典2007版附录Ⅷ B 欧洲药典第5版2.2.19-2014 氮测定法美国药典第31版<461>英国药典2007版附录Ⅷ H 欧洲药典第5版2.5.915 硫酸盐检查法中国药典2005 年版二部附录Ⅷ B 美国药典第31版<221>英国药典2007版附录Ⅶ欧洲药典第5版2.4.1316 硒检查法中国药典2005版二部附录Ⅷ D 美国药典第31版<291>17 铁盐检查法中国药典2005版一部附录Ⅸ D、二部附录Ⅷ G美国药典第31版<241> 英国药典2007版附录Ⅶ欧洲药典第5版2.4.918 重金属检查法美国药典第31版<231>英国药典2007版附录Ⅶ欧洲药典第5版2.4.819 砷盐检查法美国药典第31版<211>20 铵盐检查法中国药典2005版二部附录Ⅷ K 英国药典2007版附录Ⅶ欧洲药典第5版2.4.121 干燥失重检查法中国药典2005版一部附录Ⅸ G、二部附录Ⅷ L美国药典第31版<731> 英国药典2007版附录Ⅸ D欧洲药典第5版2.2.3222 炽灼残渣检查法中国药典2005 年版一部附录ⅨJ、二部附录ⅧN美国药典第31版<281> 英国药典2007版附录XI J欧洲药典第5版2.4.1623 有机溶剂残留量测定法美国药典第31版<467>24 溶液颜色检查法中国药典2005版一部附录Ⅺ、二部附录Ⅸ A美国药典第31版<631>英国药典2007版附录ⅣB欧洲药典第5版2.2.2不做中国药典2005版第三法25 氯化物检查法中国药典2005年版一部附录（ⅨC）/二部附录（Ⅷ A）美国药典第31版<221>英国药典2007年版附录Ⅶ欧洲药典第5版2.4.426 容量分析测定中国药典2005年版二部/一部美国药典第31版英国药典2007年版27 水分测定法中国药典2005版一部附录Ⅸ H、二部附录Ⅷ M 美国药典第31版<921>英国药典2005版附录Ⅸ C欧洲药典第5版2.5.32欧洲药典第5版2.5.12欧洲药典第5版2.2.13不做中国药典2005版第二法鉴别测试<181> Identification - Organic Nitrogenous Bases 鉴别-含有机氮<191> Identification Test - General 普通鉴别<193> Identification - Tetracyclines 鉴别-四环素<197> Spectrophotometric Identification Tests FTIR 红外鉴别UV 紫外鉴别限度测试<211> Arsenic 砷<221> Chloride and Sulfate 氯和硫<223> Dimethylaniline 二甲基苯胺<231> heavy metal Method Ⅰ重金属Ⅰ法Method Ⅱ重金属Ⅱ法Method Ⅲ重金属Ⅲ法<241> Iron 铁<251> Lead 铅<271> Readily Carbonizable Substances Test 易炭化物<281> Residue on Ignition 灼烧残渣<291> Selenium 硒其他测试及含量<301> Acid - neutralizing Capacity 酸度<391> Epinephrine assay 肾上腺素含量<401> Fats and Fixed Oils 脂肪和硬化油<411> Folic Acid Assay 叶酸含量<425> Iodometric Assay - Antibiotics 碘量法测抗生素含量<451> Nitrite Titration 亚硝酸滴定<461> Nitrogen determination 定氮<466> Ordinary Impurities 测杂质<467> Organic Volatile Impurities 挥发性有机杂质<467> Residue Solvents 残留溶剂<471> Oxygen Flask Combustion 氧瓶燃烧法<541> Titrimetry 滴定分析法<571> Vitamin A assay 维生素A含量物理实验测定<611> Alcohol Determination 乙醇检测<621> Chromatography 色谱法HPLC 高校液相色谱GC 气相色谱TLC 薄层色谱<631> Color and achromicity 色度<641> Completeness of Solution 溶液澄清度<645> Water Conductivity 水电导率<695> Crystalline 结晶度<721> Distilling range 蒸馏范围<731> loss on drying 干燥失重<733> Loss on Ignition 灼烧失重<741> Melting Range or Temperature 熔程<776> Optical Microscopy 光学显微<781> Optical Rotation 旋光<791> pH pH值<831> Refrctive index 折射率<841> Specific Gravity 比重<851> Spectrophotometry 分光光度法FTIR 红外UV/Vis 紫外/可见光<911> Viscosity 粘度<921> water 水分。

药典翻译USP29-621色谱法中文译稿

USP29-621 色谱法<621>色谱法本章内容包括在色谱仪中使用的术语和操作法，并且提供了全面的信息。

原料药和制剂的色谱操作法的具体要求，包括吸附剂和展开剂，将在个论中给出。

色谱法是指溶质在一个由两相或多相组成的系统中按照不同的动态迁移过程使之分离的方法，每种物质在给定的方向不断的迁移，并且不同的物质由于具有不同的吸附、分配、溶解性、蒸汽压、分子大小或离子强度使之呈现出不同的迁移率。

这样分离得到的每种物质可以通过分析方法得到鉴定或测定。

一般的色谱技术需要溶质在不同的两相中进行分配，其中一相是固定的（固定相），另一相是流动的（流动相）。

流动相使溶质在固定相中流过，使之与流出更早或更晚的其它溶质呈现分离状态。

一般地，溶质借助于被称为“洗脱液”的液体或气体流从固定相中转移出。

固定相可以表现为吸附作用，例如活性氧化铝、硅胶的吸附作用，或可以通过溶解溶质起作用，将之在固定相和流动相之间分配。

在后者的过程中，被涂抹在惰性支撑物上的液体，通过化学键合在硅胶上的液体，以及直接在熔融的硅毛细管壁上的液体被作为固定相。

在气液色谱、纸色谱和各种形式的柱色谱以及被指定为即液-液分离的薄层色谱中，分配是主要的分离机理。

实际上，分离经常是吸收和分配作用相结合的结果。

其它的分离原理包括离子交换、离子对形成、分子排阻、疏水效应以及手性识别。

在USP操作法中所使用的在定性和定量分析方面有用的色谱方法有柱色谱法、气相色谱法、纸色谱法、薄层色谱法(包括高效薄层色谱)和加压液相色谱法（通常也被称为高压或高效液相色谱法）。

纸色谱和薄层色谱法由于其方便性和简单性通常用于鉴定的目的；柱色谱法提供了更宽的固定相选择机会，并且在从混合物中分离单个化合物以及定量方面是很有用的；现代的高效薄层色谱、气相色谱法和加压液相色谱法需要更加精细的装置，通常可以提供高的分离度，并鉴定和定量非常少量的物质。

在鉴别试验中标准物质的使用用于鉴别试验的标准物质的使用—在纸色谱和薄层色谱法中，某一给定的化合物在介质中从基线迁移的距离（用吸收最强的斑点的位置进行测量）与流动相前沿的迁移距离的比例，被称为化合物的R F值。

美国药典——精选推荐

美国药典──羟丙基甲基纤维素CA登记号[9004-65-3]原文页号：774-775羟丙基甲基纤维素是甲基纤维素的丙二醇醚，当在105 ℃下干燥2h，其所含的甲基团（-OCH3）和羟丙氧基团（－OCH 2CHOHCH3）符合附表所列羟丙基甲基纤维素品种的范围。

包装及储存─保存在密封良好的容器中。

标签─标签应表明取代类型及粘度类型（2%水溶液的粘度）鉴别─A：将1g样品轻轻加到装有100ml水的烧杯的水面上，让其在水表面上分散，轻敲烧杯上部，使样品均匀分散，将烧杯放置一段时间，直到杯中物变透明及有粘性（大约需要5h），摇晃烧杯以润湿剩余物，放入一搅棒，搅拌至溶解完毕，当加入一份与溶液等体积的1N氢氧化钠或1N盐酸时，溶液保持稳定状态。

B：将1g 样品加到100ml沸水中，搅拌之，形成淤浆，但粉末料并未溶解，将淤浆冷至20℃，搅拌之，所得液体清彻或者呈乳白色胶状。

C：将数毫升上述B款所得混合物滴到玻璃板上，让水蒸发，得到一自生的薄膜。

表观粘度在一已称重过的250ml 广口离心瓶中放入准确称量过的相当于2g干物质样品，将98g予先加热到80～90℃的水一并加入，用推进式搅拌器搅拌10min，将瓶置于冰浴中，继续搅拌，让瓶在冰浴中保留40min，以保证水合作用，得到完全溶解，如果必要时，将溶液重量调整到100g，将溶液离心以排除可能带进溶液的空气，将溶液温度调整到20±0.1℃，在合适的乌氏（Ubbelohde）粘度计中测定粘度（粘度计参见[911]纤维素衍生物之粘度条目）。

对于标签所标100厘泊以下之产品，测定的粘度应不小于80.0%及不大于120.0%标签值，对于标签所标高于100厘泊之产品，测定的粘度应不小于75. 0% 以及不大于140.0%标签值。

干燥失重[731]─在105℃下干燥2h，失重不大于5.0%。

燃烧后残渣[281]─对于标签粘度值大于50 厘泊之羟丙基甲基纤维素，应不大于1.5%；对于标签粘度值为50厘泊更低之产品，燃烧后残渣应不大于3%；对于1828（型）羟丙基甲基纤维素，不论什么标签粘度值，燃烧后残渣应不大于5%。

美国药典-中英文对照(翻译资料)

美国药典－中英文对照译文美国药典中记载的辣椒碱资料辣椒碱（辣椒素）分子结构式：C18H27NO3，分子量：305.41，化学名：（反）－N－[（4－N－羟基－3－甲氧基苯基）－甲基]－8－甲基－6－壬烯基酰胺以干燥提取物计算，辣椒碱含辣椒二萜类化合物总量为标示量的90％－100%,其中辣椒素的含量达到50％以上，辣椒素和二氢辣椒素总量超过75％，其它辣椒素类化合物总量不足15％。

注意事项：小心处置辣椒碱，谨防吸入辣椒碱微粒，勿使身体接触辣椒碱。

包装贮藏：密封包装，置避光，阴凉处保存。

标示量：以辣椒二萜类化合物总百分含量表示。

美国药典参考标准：美国药典辣椒素标准规范，美国药典二氢辣椒素标准规范。

鉴别：配制1.0mg/ml辣椒碱甲醇溶液，配制符合美国药典标准的辣椒碱1.0mg/ml甲醇溶液作为对照液，分别点样于0.25mm厚硅胶、凝胶混合薄层板上，点样量为10礚，将薄层板放于乙醚－甲醇（19:1）展开剂中展开，待展开剂前沿至薄层板3/4处时将薄层板取出，晾干，用0.5% 2,6-二溴苯醌-氯化亚胺甲醇溶液喷雾显色，放于氨气中片刻，取出，鉴别色谱图：供试液主要斑点颜色（兰色）及R值与对照液主要斑点颜色（兰色）及R值一致。

熔点〈741〉: 57°－66°, 一般熔融起始温度至结束温度温差不超过5°。

干燥失重〈731〉: 置40°P2O5真空干燥器中干燥5小时，失重不超过1.0%。

灼烧残渣：≤1.0％。

辣椒素，二氢辣椒素及其它辣椒二萜类化合物含量测定：流动相：磷酸水溶液（l ：1000，V/V）：乙腈(600:400)混匀，0.5祄微孔滤膜滤过，脱气。

流动相视色谱行为可作适当调整。

辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.1 mg/mL的辣椒甲醇溶液。

二氢辣椒素对照液：精密称取美国药典标准的辣椒碱适量溶于甲醇中，配制约0.025mg/mL的辣椒甲醇溶液。

USP 通则 61 62 71 1225 1226

<1225>V ALIDATION OF COMPENDIAL PROCEDURES药典规程的验证Test procedures for assessment of the quality levels of pharmaceutical articles are subject to various requirements. According to Section 501 of the Federal Food, Drug, and Cosmetic Act, assays and specifications in monographs of the United States Pharmacopeia and the National Formulary constitute legal standards. The Current Good Manufacturing Practice regulations [21 CFR 211.194(a)] require that test methods, which are used for assessing compliance of pharmaceutical articles with established specifications, must meet proper standards of accuracy and reliability. Also, according to these regulations [21 CFR 211.194(a)(2)], users of analytical methods described in USP-NF are not required to validate the accuracy and reliability of these methods, but merely verify their suitability under actual conditions of use. Recognizing the legal status of USP and NF standards, it is essential, therefore, that proposal for adoption of new or revised compendial analytical procedures be supported by sufficient laboratory data to document their validity.用于评价药物质量水平的测试规程受到多种要求的影响。

复方新诺明片美国药典标准

复方新诺明片甲氧苄氨嘧啶和磺胺甲噁唑含量：甲氧苄氨嘧啶含量：92.5~107.5%磺胺甲噁唑含量：92.5~107.5%储存：密封、避光保存鉴别：供试品溶液：将相当于含有甲氧苄氨嘧啶（4mg）的片剂粉末加入到10ml容量瓶中，再加入甲醇8ml，加温摇匀。

冷却，甲醇稀释至10ml，混匀，稍稍离心。

对照品溶液：将甲氧苄氨嘧啶（USPRS）用甲醇制成0.4mg/ml的溶液；将磺胺甲噁唑（USPRS）用甲醇制成0.2mg/ml的溶液。

点样量：5μl薄层板：薄层色谱硅胶板展距：3cm流动相：氯仿/异丙醇/二乙胺（6:5:1）干燥：暖空气中干燥。

检验：短波长紫外光检视。

结果判定：供试品溶液色谱图中甲氧苄氨嘧啶和磺胺甲噁唑的R F值与标准品一致。

溶解度：溶解介质：0.1N盐酸溶液，900ml仪器2：75转/分钟时间：60分钟检测：根据甲氧苄氨嘧啶和磺胺甲噁唑的溶解量，运用含量测定的检测方法，进行必须的容量校正（见色谱分析法621）。

根据对照品溶液中的相应峰，计算出各个活性成分的溶解度。

限值：在60分钟内，不低于70%的C10H11N3O3S和C14H18N4O3溶解。

含量均匀度(905)：符合要求。

含量测定：流动相、对照品溶液、色谱分析系统与甲氧苄氨嘧啶和磺胺甲噁唑口服混悬液一致。

供试品溶液：将不少于20只片剂粉碎、称重。

称取相当于160mg磺胺甲噁唑的粉末至100ml 容量瓶，加入甲醇50ml，用声波处理，摇匀5分钟。

冷却至室温，甲醇稀释至100ml，混匀，过滤。

取5.0ml滤液至50ml容量瓶，用流动相定容，混匀。

检测：分别检测对照品溶液和供试品溶液约（20μl），记录色谱图，测量主峰面积。

根据公式1000C(r U / r S) 计算出检测片剂粉末中C10H11N3O3S和C14H18N4O3的质量（mg）；C 是对照品溶液的浓度（mg/ml），r U和r S分别为供试品溶液和对照品溶液的峰面积。

甲氧苄氨嘧啶和磺胺甲噁唑口服混悬液的含量检测：流动相：将1400ml水、400ml乙腈、2.0ml三乙胺加至2000ml容量瓶中，用0.2N氢氧化钠和1%乙酸调节pH为5.9±0.1。

USP美国药典,二甘醇、乙二醇及其他杂质

GlycerinC 3H 8O 3 92.101,2,3-Propanetriol.Glycerol [56-81-5].» Glycerin contains not less than 99.0 percent and not more than 101.0 percent of C 3H 8O 3, calculated on the anhydrous basis. The amount of any individual impurity, excluding diethylene glycol and ethylene glycol, if detected, meets the requirements under Other Impurities (NMT 0.1%) and the amount of total impurities, including diethylene glycol and ethylene glycol, is NMT 1.0%. Packaging and storage— Preserve in tight containers.USP Reference standards 11— USP Diethylene Glycol RS . USP Ethylene Glycol RS . USP Glycerin RS .Color— Its color, when viewed downward against a white surface in a 50-mL color-comparison tube, is not darker than the color of a standard made by diluting 0.40 mL of ferric chloride CS with water to 50 mL and similarly viewed in a color-comparison tube of approximately the same diameter and color as that containing the Glycerin.Identification— [NOTE—Compliance is determined by meeting the requirements for both Identification A and B .]A: Infrared Absorption 197F .B: Standard stock solution 1—Transfer 50 mg of USP Diethylene Glycol RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Standard stock solution 2— Transfer 50 mg of USP Ethylene Glycol RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Standard stock solution 3— Transfer 50 mg of USP Glycerin RS , accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Resolution solution— Transfer 5.0 mL each of Standard stock solution 1, Standard stock solution 2, and Standard stock solution 3, to a 100-mL volumetric flask, dilute withmethanol to volume, and mix.Test solution— Transfer about 5 g of Glycerin to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Chromatographic system (see Chromatography 621)— The gas chromatograph is equipped with a flame-ionization detector, a 0.53-mm × 30-m fused-silica analytical column coated with 3.0-µm G43 stationary phase. The injection port temperature is maintained at 220 and the detector temperature is maintained at 250. The carrier gas is helium with a flow rate of about 4.5 mL per minute. The split flow ratio is about 10:1. The chromatograph is programmed as follows: Initially, the column temperature is equilibratedat 100 for 4 minutes, then increased at a rate of 50 per minute to 120, and is maintained at 120 for 10 minutes. It is then increased at a rate of 50 per minute to 220, and is maintained at 220 for 6 minutes. Chromatograph the Resolution solution, and record the peak responses and retention times as directed for Procedure: the relative retention times are about 0.3 for ethylene glycol, 0.8 for diethylene glycol, and 1.0 for glycerin; and the relative standard deviation for replicate injections for the diethylene glycol is not more than 10%.Procedure— Separately inject equal volumes (about 1 µL) of the Resolution solution and the Test solution into the chromatograph, and record the chromatograms. If a peak at the relative retention time for the diethylene glycol or ethylene glycol is present in the Test solution, the peak must be identifed and quantified as directed in the test for Diethylene glycol and ethylene glycol impurities.Specific gravity 841: not less than 1.249.Residue on ignition 281—Heat 50 g in an open, shallow 100-mL porcelain dish until it ignites, and allow it to burn without further application of heat in a place free from drafts. Cool, moisten the residue with 0.5 mL of sulfuric acid, and ignite to constant weight: the weight of the residue does not exceed 5 mg (0.01%).Water, Method I 921: not more than 5.0%.Chloride 221—A 7.0-g portion shows no more chloride than corresponds to 0.10 mL of 0.020 N hydrochloric acid (0.001%).Sulfate 221—A 10-g portion shows no more sulfate than corresponds to 0.20 mL of 0.020 N sulfuric acid (about 0.002%).Heavy metals 231—Mix 4.0 g with 2 mL of 0.1 N hydrochloric acid, and dilute with water to 25 mL: the limit is 5 µg per g.Limit of chlorinated compounds— Accurately weigh 5 g of Glycerin into a dry, round-bottom, 100-mL flask, add 15 mL of morpholine, and connect the flask by a ground joint to a reflux condenser. Reflux gently for 3 hours. Rinse the condenser with 10 mL of water,receiving the washing in the flask, and cautiously acidify with nitric acid. Transfer the solution to a suitable comparison tube, add 0.50 mL of silver nitrate TS, dilute with water to 50.0 mL, and mix: the turbidity is not greater than that of a blank to which 0.20 mL of 0.020 N hydrochloric acid has been added, the refluxing being omitted (0.003% of Cl).Fatty acids and esters— Mix 50 g of Glycerin with 50 mL of freshly boiled water and 5 mL of 0.5 N sodium hydroxide VS, boil the mixture for 5 minutes, cool, add phenolphthalein TS, and titrate the excess alkali with 0.5 N hydrochloric acid VS. Performa blank determination (see Residual Titrations under Titrimetry 541): not more than 1 mL of 0.5 N sodium hydroxide is consumed.Diethylene glycol and ethylene glycol impurities—Internal standard solution— Transfer 100 mg of 2,2,2-trichloroethanol (internal standard), accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Standard stock solution 1— Transfer 50 mg of USP Diethylene Glycol RS, accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Standard stock solution 2— Transfer 50 mg of USP Ethylene Glycol RS, accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Standard stock solution 3— Transfer 50 mg of USP Glycerin RS, accurately weighed, to a 100-mL volumetric flask, dilute with methanol to volume, and mix.Standard solution— Transfer 5.0 mL each of Standard stock solution 1, Standard stock solution 2, and the Internal standard solution to a 100-mL volumetric flask, and dilute with methanol to volume, and mix.Resolution solution— Transfer 500 mg of USP Glycerin RS to a 10-mL volumetric flask, add 0.5 mL each of Standard stock solution 1 and Standard stock solution 2, dilute with methanol to volume, and mix.Test solution— Transfer about 5 g of Glycerin to a 100-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with methanol to volume, and mix.Chromatographic system (see Chromatography 621)— The gas chromatograph is equipped with a flame-ionization detector, a 0.53-mm × 30-m fused-silica analytical column coated with 3.0-µm G43 stationary phase. The injection port temperature is maintained at 220 and the detector temperature is maintained at 250. The carrier gas is helium, flowing at a rate of about 4.5 mL per minute. The split flow ratio is about 10:1. The chromatograph is programmed as follows. Initially, the column temperature is equilibratedat 100 for 4 minutes, then increased at a rate of 50 per minute to 120, and is maintained at 120 for 10 minutes then increased at a rate of 50 per minute to 220, andis maintained at 220for 6 minutes. Chromatograph the Standard solution, and record thepeak response ratio and retention times as directed for Procedure: the relative retention times are about 0.3 for ethylene glycol, 0.8 for diethylene glycol, and 1.0 for glycerin; the relative standard deviation for replicate injections for the diethylene glycol is not more than 10%; and the limit of quantitation of diethylene glycol and ethylene glycol is not more than 0.025%.Procedure— Separately inject equal volumes (about 1 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the responses for the ethylene glycol and diethylene glycol peaks. Calculate the percentage of diethylene glycol and ethylene glycol in the portion of Glycerin taken by the formula:100(CS / CU)(RU/ RS)in which CSis the concentration, in mg per mL, of diethylene glycol (or ethylene glycol) inthe Standard solution; CUis the concentration, in mg per mL, of Glycerin in the Testsolution; and RU and RSare the peak response ratios for diethylene glycol (or ethyleneglycol) to the internal standard peak obtained from the Test solution and the Standard solution: NMT the limit of quantitation for each, is found (0.025%).Assay—Sodium periodate solution— Dissolve 60 g of sodium metaperiodate in sufficient water containing 120 mL of 0.1 N sulfuric acid to make 1000 mL. Do not heat to dissolve the periodate. If the solution is not clear, pass through a sintered-glass filter. Store the solution in a glass-stoppered, light-resistant container. Test the suitability of this solution as follows. Pipet 10 mL into a 250-mL volumetric flask, dilute with water to volume, and mix. To about 550 mg of Glycerin dissolved in 50 mL of water add 50 mL of the diluted periodate solution with a pipet. For a blank, pipet 50 mL of the solution into a flask containing 50 mL of water. Allow the solutions to stand for 30 minutes, then to each add 5 mL of hydrochloric acid and 10 mL of potassium iodide TS, and rotate to mix. Allow to stand for 5 minutes, add 100 mL of water, and titrate with 0.1 N sodium thiosulfate, shaking continuously and adding 3 mL of starch TS as the endpoint is approached. The ratio of the volume of 0.1 N sodium thiosulfate required for the glycerin–periodate mixture to that required for the blank should be between 0.750 and 0.765.Procedure— Transfer about 400 mg of Glycerin, accurately weighed, to a 600-mL beaker, dilute with 50 mL of water, add bromothymol blue TS, and acidify with 0.2 N sulfuric acid to a definite green or greenish yellow color. Neutralize with 0.05 N sodium hydroxide to a definite blue endpoint, free from green color. Prepare a blank containing 50 mL of water, and neutralize in the same manner. Pipet 50 mL of the Sodium periodate solution into each beaker, mix by swirling gently, cover with a watch glass, and allow to stand for 30minutes at room temperature (not exceeding 35) in the dark or in subdued light. Add 10 mL of a mixture of equal volumes of ethylene glycol and water, and allow to stand for 20 minutes. Dilute each solution with water to about 300 mL, and titrate with 0.1 N sodiumhydroxide VS to a pH of 8.1 ± 0.1 for the specimen under assay and 6.5 ± 0.1 for the blank, using a pH meter. Each mL of 0.1 N sodium hydroxide, after correction for the blank, is equivalent to 9.210 mg of C 3H 8O 3.Auxiliary Information— Please check for your question in the FAQs before contacting USP.USP32–NF27 Page 2513Pharmacopeial Forum : Volume No. 28(4) Page 1245Chromatographic Column— GLYCERINChromatographic columns text is not derived from, and not part of, USP 32 or NF 27. Topic/Question Contact Expert Committee Monograph Kevin T. Moore, Ph.D.Scientist1-301-816-8369(EM105) Excipient Monographs 1Reference StandardsLili Wang, Technical ServicesScientist1-301-816-8129RSTech@。

美国药典36版目录

<681>
固体的疏松密度和叩击密度测定
色谱法呈色与消色溶解的完全性检查总有机炭测定水导电性测定冻凝温度的测定包转和贮藏要求玻璃容器塑料容器附加包装构成容器性能检测
用于无菌固体和液体溶剂形式的单独单位容器和单位剂量容器的重新分配
<691> 棉花
<695> <696> <698>
<55>
生物指示剂：耐受性能检测
<61>
非无菌制品的微生物检查：计数试验
<62>
非无菌制品的特定菌检查
<63>
支原体检测
<71>
无菌检测
生物学试验和检定
<81>
抗生素微生物检定
<85>
细菌内毒素检测
如大肠杆菌、金葡菌、沙门氏菌等
<87>
体外生物反应性试验
<88>
体内生物反应性试验
<90> <91> <92> <111> <115> <121> <123> <130> <151>
美国药典目录
检测和含量分析的一般要求
<1>
注射剂
<3>
局部和经皮的药物产品-产品质量检测
<11>
USP对照标准品
检测和含量分析的仪器
<16>
自动分析方法
<17>
处方容器具标签
<21>
测温仪

美罗培南_美国药典

USP 35Official Monographs / Meropenem3813C U= nominal concentration of mercaptopurine in the essary correction. Each mL of 0.1 N hydrochloric acid is equiva-Sample solution (mg/mL)lent to 12.60 mg of Hg(NH2)Cl.F= relative response factor for each individualimpurity (see Table 2)Acceptance criteriaIndividual impurities: See Table 2. [N OTE—Disregard any Meropenemimpurity peak less than 0.05%.]Table 2Relative Relative AcceptanceRetention Response Criteria,Name Time Factor NMT (%)Didanosine relatedC17H25N3O5S·3H2O437.52compound A a0.54 6.30.31-Azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid, 3-[[5-Mercaptopurine 1.00——[(dimethylamino)carbonyl]-3-pyrrolidinyl]thio]-6-(1-hydroxy-Mercaptopurine ethyl)-4-methyl-7-oxo, trihydrate, [4R-disulfide b 2.90 4.40.4[3(3S*,5S*),4α,5β,6β(R*)]]-.Any unspecified—(4R,5S,6S)-3-[[(3S,5S)-5-(Dimethylcarbamoyl)-3-pyrrolidinyl]thio] impurity 1.00.2-6-[(1R)-1-hydroxyethyl]-4-methyl-7-oxo-1-azabicyclo[3.2.0] Total impurities——0.6hept-2-ene-carboxylic acid, trihydrate [119478-56-7].a Hypoxanthine.Anhydrous383.47 [96036-03-2].b1,2-Di(9H-purin-6-yl)disulfane.» Meropenem contains not less than 98.0 per-v USP35cent and not more than 101.0 percent ofC17H25N3O5S, calculated on the anhydrous basis. ADDITIONAL REQUIREMENTS•P ACKAGING AND S TORAGE: Preserve in well-closed containers.Packaging and storage—Preserve in tight containers. Store •L ABELING: When more than one Dissolution test is given, thethe dry powder at controlled room temperature.labeling states the Dissolution test used only if Test 1 is notLabeling—Where it is intended for use in preparing injectable used.dosage forms, the label states that it is sterile or must be sub-•USP R EFERENCE S TANDARDS〈11〉jected to further processing during the preparation of injectable USP Mercaptopurine RSdosage forms.USP Reference standards 〈11〉—USP Endotoxin RSAmmoniated MercuryUSP Meropenem RSIdentification—Hg(NH2)Cl252.07A: Infrared Absorption 〈197K〉.Mercury amide chloride.Mercury amide chloride [10124-48-8].B: Ultraviolet Absorption 〈197U〉—Solution:30 µg per mL.» Ammoniated Mercury contains not less thanMedium:water.98.0 percent and not more than 100.5 percentSpecific rotation 〈781〉:between −17° and −21°, measured of Hg(NH2)Cl.at 20°.Test solution: 5 mg per mL, in water.Packaging and storage—Preserve in well-closed, light-resis-tant containers.pH 〈791〉: between 4.0 and 6.0, in a solution (1 in 100). Identification—Water, Method Ic 〈921〉:between 11.4% and 13.4%.A: A 0.1-g portion is soluble, with the evolution of ammo-Residue on ignition 〈281〉: not more than 0.1%, igniting at nia, in a cold solution of 1g of sodium thiosulfate in 2 mL of500±50°, instead of at 800±25°. Use a desiccator containing water. When this solution is heated gently, a rust-colored mix-silica gel.ture is formed, from which a red precipitate is obtained on Heavy metals—centrifugation. If the solution is strongly heated, a black mixture Sodium sulfide reagent—Dissolve 5g of sodium sulfide in a forms.mixture of 10 mL of water and 30 mL of glycerin. Preserve in B: When heated with 1N sodium hydroxide, it becomes yel-well-filled, light-resistant bottles, and use within 3 months. low, and ammonia is evolved.Test solution—Transfer 1.0 g of Meropenem to a quartz or C: A solution in warm acetic acid yields with potassium io-porcelain crucible, cover loosely with a lid, and carbonize by dide TS a red precipitate, which is soluble in an excess of the gentle ignition. After cooling, add 2 mL of nitric acid and 5 reagent. The solution yields a white precipitate with silver ni-drops of sulfuric acid, heat cautiously until white fumes evolve, trate TS.and incinerate by ignition at 500° to 600°. Cool, add 2 mL of Residue on ignition 〈281〉: not more than 0.2%.hydrochloric acid, and evaporate on a water bath to dryness.Moisten the residue with 3 drops of hydrochloric acid, add 10 Mercurous compounds—Dissolve 2.5 g in 25 mL of warmmL of hot water, and warm for 2 minutes. Add 1 drop of phe-hydrochloric acid, filter through a tared filtering crucible, washnolphthalein TS, add ammonia TS, dropwise, until the solution with water, and dry at 60° to constant weight: the weight ofdevelops a pale red color, and add 2 mL of 1N acetic acid.the residue does not exceed 5 mg (0.2%).Filter, if necessary, to obtain a clear solution, washing the filter Assay—Mix about 0.25 g of Ammoniated Mercury, accuratelywith 10 mL of water. Transfer the filtrate and the washing to a weighed, with about 10 mL of water. Add 3g of potassium50-mL color-comparison tube, and add water to obtain a vol-iodide, mix occasionally until dissolved, and add about 40 mLume of 50 mL.of water. Add methyl red TS, and titrate with 0.1 N hydrochlo-Standard solution—Evaporate a mixture of 2 mL of nitricric acid VS. Perform a blank determination, and make any nec-acid, 5 drops of sulfuric acid, and 2 mL of hydrochloric acid ona water bath, further evaporate to dryness on a hot sand bath,3814Meropenem / Official Monographs USP 35and moisten the residue with 3 drops of hydrochloric acid. Pro-than 1.5; and the relative standard deviation for replicate injec-ceed as directed for Test solution, beginning with “add 10 mL tions is not more than 2.0%.of hot water,” except add water to obtain a volume of 49 mL.Procedure—Separately inject equal volumes (about 10 µL) of Add 1.0 mL of Standard Lead Solution (see Heavy Metals 〈231〉).the Standard solution and the Test solution into the chromato-Procedure—To the tubes containing the Test solution and the graph, record the chromatograms, using a period of chroma-Standard solution, add 1 drop of Sodium sulfide reagent, mix,tography for the Test solution that is about 3 times the retention and allow to stand for 5 minutes. The color in the tube contain-time of meropenem, and measure the peak responses. Major ing the Test solution is not darker than the color in the tube impurity peaks may be observed at retention times of about containing the Standard solution (0.001%).0.45 and 1.9 in relation to the retention time of meropenem.Calculate the percentage of each impurity in the chromatogram Limit of acetone—obtained from the Test solution by the formula: Internal standard solution—Prepare a solution in dimethyl-formamide containing 0.05 µL of ethyl acetate per mL.(CS/C U)(P)(r i/r S) Standard solution—Transfer about 50 mg of acetone, accu-rately weighed, to a 100-mL volumetric flask, dilute with di-in which CS is the concentration, in mg per mL, of USP Mer-methylformamide to volume, and mix. To 1.0 mL of this solu-openem RS in the Standard solution; CU is the concentration, in tion, add 10.0 mL of the Internal standard solution, and mix.mg per mL, of Meropenem in the Test solution; P is the statedTest solution—Dissolve 100 mg of Meropenem, accurately percentage, calculated on the anhydrous basis, of meropenem weighed, in 0.2 mL of dimethylformamide and 2.0 mL of Inter-in USP Meropenem RS; r i is the peak response of any individual nal standard solution.impurity obtained from the Test solution; and r S is the peak re-sponse of meropenem obtained from the Standard solution. Not Chromatographic system (see Chromatography 〈621〉)—Themore than 0.3% of any of two major impurities is found, calcu-gas chromatograph is equipped with a flame-ionization detectorlated on the anhydrous basis; not more than 0.1% of any other and a 3-mm × 2-m column that contains support S2 and isimpurity is found, calculated on the anhydrous basis; and the maintained at a constant temperature of about 150°. The injec-sum of all such other impurities is not more 0.3%.tion port temperature is maintained at about 170°. Nitrogen isthe carrier gas, with the flow rate adjusted so that the retention Other requirements—Where the label states that Mer-time for acetone is about 3 minutes.openem is sterile, it meets the requirements for Sterility 〈71〉and for Bacterial endotoxins under Meropenem for Injection.Procedure—Separately inject equal volumes (about 2 µL) ofWhere the label states that Meropenem must be subjected to the Standard solution and the Test solution into the chromato-further processing during the preparation of injectable dosage graph, record the chromatograms, and measure the peak re-forms, it meets the requirements for Bacterial endotoxins under sponses for the acetone peak and the internal standard peak.Meropenem for Injection.Calculate the percentage of acetone in the portion of Mer-openem taken by the formula:Assay—Diluted phosphoric acid—Dilute 10 mL of phosphoric acid (W A/5W U)(R U/R S)with water to make 100 mL of solution.Solvent—Transfer 1.0 mL of triethylamine to a 1000-mL volu-in which W A is the weight, in mg, of acetone in the Standard metric flask containing 900 mL of water. Adjust with Dilutedsolution; W U is the quantity, in mg, of Meropenem in the Test phosphoric acid to a pH of 5.0 ± 0.1, dilute with water to vol-solution; and R U and R S are the peak area ratios of acetone to ume, and mix.the internal standard obtained from the Test Solution and theMobile phase—Prepare a mixture of Solvent and methanol Standard solution, respectively. Not more than 0.05% is found.(5:1). Make adjustments if necessary (see System Suitability Chromatographic purity—under Chromatography 〈621〉).Diluted phosphoric acid—Dilute 10 mL of phosphoric acid Standard preparation—Transfer about 25 mg of USP Mer-with water to make 100 mL of solution.openem RS, accurately weighed, to a 50-mL volumetric flask, Solvent—Transfer 1.0 mL of triethylamine to a 1000-mL volu-add Solvent, swirl to dissolve, dilute with Solvent to volume, and metric flask containing 900 mL of water. Adjust with Diluted mix. [NOTE—Immediately after preparation, store this solution in phosphoric acid to a pH of 5.0 ± 0.1, dilute with water to vol- a refrigerator. It may be used for 24 hours.]ume, and mix.Assay preparation—Transfer about 25 mg of Meropenem, ac-Mobile phase—Transfer 1.0 mL of triethylamine to a 1000-mL curately weighed, to a 50-mL volumetric flask, add Solvent, swirl volumetric flask containing 900 mL of water. Adjust with Diluted to dissolve, dilute with Solvent to volume, and mix. Use this phosphoric acid to a pH of 5.0 ± 0.1, dilute with water to vol-solution immediately after preparation.ume, and mix. Mix this solution with 70 mL of acetonitrile.Chromatographic system (see Chromatography 〈621〉)—The Make adjustments if necessary (see System Suitability under liquid chromatograph is equipped with a 300-nm detector and Chromatography 〈621〉). a 4.6-mm × 25-cm column that contains 5-µm packing L1. Ad-Standard solution—Prepare a solution of USP Meropenem RS just the flow rate so that the retention time for meropenem is in Solvent having a known concentration of about 0.025 mg of about 6 to 8 minutes. The flow rate is about 1.5 mL per min-USP Meropenem RS per mL. [NOTE—Immediately after prepara-ute. Chromatograph the Standard preparation, and record the tion, store this solution in a refrigerator and use within 24peak responses as directed for Procedure: the column efficiency hours.]is not less than 2500 theoretical plates; the tailing factor is not Test solution—Dissolve an accurately weighed quantity of more than 1.5; and the relative standard deviation for replicate Meropenem quantitatively in Solvent to obtain a solution having injections is not more than 2.0%.a known concentration of about 5 mg per mL. Use this Test Procedure—Separately inject equal volumes (about 5 µL) of solution immediately.Standard preparation and Assay preparation into the chromato-Chromatographic system (see Chromatography 〈621〉)—The graph, record the chromatograms, and measure the areas for liquid chromatograph is equipped with a 220-nm detector and the major peaks. Calculate the quantity, in mg, of C17H25N3O5S a 4.6-mm × 25-cm column that contains 5-µm packing L1 and in the portion of Meropenem taken by the formula:is maintained at a constant temperature of about 40°. The flowrate is about 1.6 mL per minute, and is adjusted so that the(W S/W U)(P)(r U/r S)retention time of meropenem is between 5 and 7 minutes.Chromatograph the Standard solution, and record the peak re-in which W S is the weight, in mg, of USP Meropenem RS taken sponses as directed for Procedure: the column efficiency is not to prepare the Standard preparation, calculated on the anhy-less than 2500 theoretical plates; the tailing factor is not more drous basis; W U is the weight, in mg, of Meropenem taken toprepare the Assay preparation; P is the stated percentage, calcu-USP 35Official Monographs / Meropenem 3815lated on the anhydrous basis, of meropenem in USP Mer-than 0.8% of the impurity, if any, with a retention time of openem RS; and r U and r S are the meropenem peak responses about 0.45 relative to that of meropenem, is found; and not obtained from the Assay preparation and the Standard prepara-more than 0.6% of the impurity, if any, with a retention time tion, respectively.of about 1.9 relative to that of meropenem, is found.Content of sodium—Potassium chloride solution—Transfer 38.1 g of potassium chloride to a 1000-mL volumetric flask, dissolve in and dilute with water to volume, and mix.Meropenem for InjectionStandard sodium solution—Dissolve 25.42 mg of sodium chloride, previously dried at 105° for 2 hours and accurately » Meropenem for Injection is a sterile dry mixture weighed, quantitatively in water to obtain a solution having a of Meropenem and Sodium Carbonate. It con-concentration of 25.42 µg of sodium chloride per mL. Transfer tains not less than 90.0 percent and not more 5.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Potassium chloride solution , dilute with water to volume, and than 120.0 percent of the labeled amount of mix.meropenem (C 17H 25N 3O 5S).Test solution—Transfer an accurately measured volume of the Packaging and storage—Preserve in tight Containers for stock solution used to prepare Assay preparation 1 or Assay Sterile Solids as described under Injections 〈1〉. Store at con-preparation 2, as appropriate, equivalent to about 25 mg of trolled room temperature.meropenem, to a 200-mL volumetric flask, dilute with water to volume, and mix. Transfer 5.0 mL of this solution to a 50-mL Labeling—It meets the requirements for Labeling under Injec-volumetric flask, add 5.0 mL of Potassium chloride solution , di-tions 〈1〉. Label it to state the quantity, in mg, of sodium (Na) in lute with water to volume, and mix.a given dosage of meropenem.Blank solution—Transfer 5.0 mL of Potassium chloride solution USP Reference standards 〈11〉—to a 50-mL volumetric flask, dilute with water to volume, and USP Endotoxin RS mix.USP Meropenem RSProcedure—Concomitantly determine the absorbances of the Constituted solution—At the time of use, it meets the re-Standard sodium solution and the Test solution at the sodium quirements for Constituted Solutions under Injections 〈1〉.emission line at 589.6 nm with an atomic absorption spectro-Identification—The retention time for the meropenem peak photometer (see Spectrophotometry and Light-Scattering 〈851〉),in the chromatogram of the Assay preparation corresponds to equipped with a sodium hollow-cathode lamp and a single-slot that in the chromatogram of the Standard preparation, as ob-burner, using an air–acetylene flame and the Blank solution as tained in the Assay.the blank. Calculate the quantity, in mg, of sodium (Na) in the constituted Meropenem for Injection by the formula:Bacterial endotoxins 〈85〉—It contains not more than 0.125USP Endotoxin Unit per mg of meropenem.(22.99/58.44)(C )(2000V/vM )(A U /A S )Sterility 〈71〉—It meets the requirements when tested as di-rected for Membrane Filtration under Test for Sterility of the Prod-in which 22.99 and 58.44 are the atomic weight of sodium and uct to be Examined.the molecular weight of sodium chloride, respectively; C is the Uniformity of dosage units 〈905〉: meets the requirements.concentration, in µg per mL, of sodium chloride in the Standard pH 〈791〉: between 7.3 and 8.3, in a solution (1 in 20).sodium solution; V is the volume, in mL, of the stock solution obtained in Assay preparation 1 or Assay preparation 2, as ap-Loss on drying 〈731〉—Dry it in vacuum at 65° for 6 hours: it propriate; v is the volume, in mL, of the portion of the stock loses between 9.0% and 12.0% of its weight.solution taken to prepare the Test solution; M is the total quan-Particulate matter 〈788〉: meets the requirements for small-tity, in mg, of meropenem in the stock solution obtained in volume injections.Assay preparation 1 or Assay preparation 2, as appropriate,Chromatographic purity—based on the result of the Assay; and A U and A S are the ab-Diluted phosphoric acid , Solvent , Mobile phase , and Chromato-sorbances of the Test solution and the Standard sodium solution,graphic system—Proceed as directed in the test for Chromato-respectively: it contains between 80% and 120% of the labeled graphic purity under Meropenem .amount of sodium.Standard solution—Prepare a solution of USP Meropenem RS Assay—in Solvent having a known concentration of about 0.029 mg of Mobile phase—Dilute 15 mL of tetrabutylammonium hydrox-USP Meropenem RS per mL. [NOTE —Immediately after prepara-ide solution (25% in water) with water to 750 mL. Adjust with tion, store this solution in a refrigerator. It may be used for 24dilute phosphoric acid (1 in 10) to a pH of 7.5 ± 0.1. Add 150hours.]mL of acetonitrile and 100 mL of methanol, mix, and degas.Test solution—Transfer an accurately weighed portion of Mer-Make adjustments if necessary (see System Suitability under openem for Injection, equivalent to about 50 mg of mer-Chromatography 〈621〉).openem, based on the labeled amount, to a 10-mL volumetric Standard preparation—Dissolve an accurately weighed por-flask, dilute with Solvent to volume, and mix. Use this Test solu-tion of USP Meropenem RS quantitatively in Mobile phase to tion immediately.obtain a solution having a known concentration of about 0.11Procedure—Proceed as directed in the test for Chromato-mg per mL. This solution contains the equivalent of about 0.1graphic purity under Meropenem . Calculate the percentage of mg of meropenem per mL. [NOTE —Immediately after prepara-each impurity in the portion of Injection taken by the formula:tion, store this solution in a refrigerator and use within 24hours.]10(CP /m )(r i /r S )Assay preparation 1 (where it is represented as being a sin-gle-dose container)—Constitute a container of Meropenem for in which C is the concentration, in mg per mL, of USP Mer-Injection with a volume of water, accurately measured, corre-openem RS in the Standard solution; P is the stated percentage,sponding to the amount of solvent specified in the labeling.calculated on the anhydrous basis, of meropenem in USP Mer-Withdraw all of the withdrawable contents, using a suitable hy-openem RS; m is the amount, in mg, of meropenem in the podermic needle and syringe, and transfer to a 100-mL volu-portion of Injection taken to prepare the Test solution , based on metric flask. Dilute with water to volume, and mix. Dilute an the label claim; r i is the peak response of any individual impu-accurately measured volume of this stock solution quantitatively rity obtained from the Test solution; and r S is the peak response with Mobile phase to obtain a solution having a concentrationof meropenem obtained from the Standard solution . Not more。

美国药典USP31-NF26色谱《621》

621CHROMATOGRAPHY色谱法INTRODUCTION介绍This chapter defines the terms and procedures used in chromatography and provides general information. Specific requirements for chromatographic procedures for drug substances and dosage forms, including adsorbent and developing solvents, are given in the individual monographs.此章节定义了色谱法中用到的术语和步骤，并提供了通用信息。

对于原料药和成药的色谱步骤的具体要求，包括吸附剂和展开溶剂，在具体各论中给出。

Chromatography is defined as a procedure by which solutes are separated by a dynamic differential migration process in a system consisting of two or more phases, one of which moves continuously in a given direction and in which the individual substances exhibit different mobilities by reason of differences in adsorption, partition, solubility, vapor pressure, molecular size, or ionic charge density. The individual substances thus separated can be identified or determined by analytical procedures.色谱法是应用溶质在两相或多相系统中的差速迁移来进行分离的技术，其中一相持续地向特定方向移动，而由于物质在吸附性、分配、溶解性、气体压力、分子大小、或离子电荷密度上的差异，会显示出不同的移动性。

USP31-621色谱法中文译稿

对于原料药和成药的色谱步骤的具体要求，包括吸附剂和展开溶剂，在具体各论中给出。

usp美国药典结构梳理

USP35-NF-30结构整理vivi2010-10-02USP总目录：1 New Official Text修订文件加快修订过程包括勘误表，临时修订声明（IRAS），修订公告。

勘误表，临时修订声明，修订公告在USP网站上New Official Text部分刊出，勘误表，临时修订公告也会在PF上刊出2front matter前言药典与处方集增补删减情况，审核人员，辅料收录情况3凡例药典，1标题和修订2 药典地位和法律认可3标准复合性4专论和通则5 专论组成6 检验规范和检验方法7 测试结果8 术语和定义9 处方和配药10 包装存储与标签4通则4.1章节列表4.2一般检查和含量测定（章节编号小于1000）检查和含量分析的一般要求检查和含量分析的仪器，微生物检查，生物检查和含量测定，化学检查和含量测定，物理检查和测定4.3一般信息（章节号大于1000）5食物补充剂通则6试剂（试剂，指示剂，溶液等）7参考表性状描述和溶解性查询表（按字母顺序）8食品补充剂各论（字母顺序）9NF各论（辅料标准）10 USP各论11术语附件：通则的章节中文目录（使用起来比较方便，直接找对应章节号即可）一、通用试验和检定（1）试验和检定的总要求1 注射剂11 参比标准物（2）试验和检定的装置16 自动分析方法21 测温仪31 容量装置，如容量瓶、移液管、滴定管，各种规格的误差限度41 砝码和天平（3）微生物学试验51 抗菌效力试验55 生物指示剂：耐受性能试验61 微生物限度试验61 非灭菌制品的微生物检查：计数试验62 非灭菌制品的特定菌检查，如大肠杆菌、金葡菌、沙门氏菌等71 无菌试验（4）生物学试验和检定81 抗生素微生物检定85 细菌内毒素试验87 体外生物反应性试验：检查合成橡胶、塑料、高聚物对哺乳类细胞培养的影响88 体内生物反应性试验：检查上述物质对小鼠、兔iv、ip或肌内植入的影响91 泛酸钙检定111 生物检定法的设计和分析115 右泛醇检定121 胰岛素检定141 蛋白质——生物适应试验，用缺蛋白饲料大鼠，观察水解蛋白注射液和氨基酸混合物的作用151 热原检查法161 输血、输液器及类似医疗装置的内毒素、热原、无菌检查171 维生素B12 活性检定（5）化学试验和检定A 鉴别试验181 有机含氮碱的鉴别191 一般鉴别试验193 四环素类鉴别197 分光光度法鉴别试验201 薄层色谱鉴别试验B 限量试验206 铝211 砷221 氯化物和硫酸盐223 二甲基苯胺226 4-差向脱水四环素231 重金属241 铁251 铅261 汞271 易炭化物试验281 炽灼残渣291 硒C 其他试验和检定301 中和酸能力311 藻酸盐检定331 苯丙胺检定341 多剂量容器注射剂中所加防腐剂含量的气相色谱或极谱法测定345 枸橼酸与其盐以及磷酸盐检定351 甾体检定361 巴比妥酸盐检定371 维生素B12放射示踪物检定381 注射剂橡胶塞检查391 肾上腺素检定401 脂肪和固定油检查411 叶酸检定425 抗生素碘量法检定429 微粒大小的光衍射测量431 甲氧基测定441 烟酸或烟酰胺检定451 亚硝酸盐滴定461 氮测定466 普通杂质的薄层色谱法检查467 有机挥发性杂质检查法467 残留溶剂测定471 氧瓶燃烧法481 核黄素检定501 有机含氮碱的盐511 单一甾醇检定521 磺胺类的色谱法检定531 硫胺检定541 滴定法554 α-生育酚检定561 植物来源物品的一般检查项目563 植物来源物品的各种鉴别项目（植物学部分、显微鉴别、化学鉴别）565 植物提取物的一般提取方法和要求571 维生素A检定：化学法、色谱法581 维生素D检定：色谱法、化学法、生物法591 锌测定（6）物理试验和测定601 气雾剂、鼻喷雾剂、计量吸入剂和干粉吸入剂的各项检测611 乙醇含量测定：蒸馏法、气一液色谱法616 固体的疏松密度和叩击密度测定621 色谱法631 色度检查和标准641 溶解的完全性检查643 总有机炭测定645 水导电性测定651 冻凝温度的测定661 药用容器的检测项目要求671 盛装胶囊和片剂容器加盖后对湿气的通透性试验691 棉花吸附性和纤维长度测定695 结晶性检查696 用溶液测热法测定结晶度698 装量检查699 固体密度（粉粒密度测定法）701 崩解试验711 溶出试验721 蒸馏温度范围（馏程）测定724 通过透皮转运系统药物的释放726 电泳727 毛细管电泳730 等离子体光谱化学检查法731 干燥失重733 炽灼失重736 质谱法741 熔点范围或温度的测定751 眼膏中的金属颗粒测定755 最低装量检查法761 核磁共振771 眼用软膏的要求776 光学显微镜微粒检查法781 旋光度检查785 渗透压摩尔浓度测定法786 用分析筛测量颗粒大小的分布788 注射液中微粒物质测定法789 眼用溶液中微粒物质测定法791 PH测定法795 非灭菌制剂的药物配制要求797 灭菌制剂的药物配制要求801 极谱法811 粉末细度测定821 放射活性药物823 正电子发射层析X线摄影（PET）所用放射性药物的配制831 折光指数测定841 比重测定846 粉末的比表面积测定851 分光光度法与光散射861 外科缝合线直径检查871 附有针的缝合线检查881 外科缝合线、纺织品与膜片的弹力强度检查891 热分析：温度变化、热解重量分析、易熔杂质分析等905 剂量单位的均匀性检查（含量均匀度、装量差异）911 黏度测定921 药品含水量的测定941 结晶型药物的X线衍射分析二、通用资料1010 数据分析方法1015 诊断用放射药的自动合成装置1031 药用容器、医用装置和植入物所用材料的生物相容性检查1035 灭菌用生物指示剂1041 生物制品的批签发1043 细胞、基因和组织工程产品的辅助材料1045 生物技术产品1046 细胞和基因治疗产品1047 生物技术产品的检验法1048 生物技术产品的质量——重组DNA蛋白质产品生产所用细胞表达构成的分析1049 生物技术产品的稳定性试验1050 人或动物来源的细胞系所得生物技术产品的病毒安全性评价1051 玻璃仪器清洗方法1061 颜色的仪器测量1065 离子色谱1072 消毒剂与防腐剂1074 赋形剂生物学安全性评价指导原则1075 复方药物配制质量规范1078 大批量药用赋形剂的生产质量规范1079 储存与运输的质量规范1081 明胶的凝胶强度1086 药品中的杂质来源1087 特性溶出1088 剂型的体外和体内评价1090 体内生物等效性试验指导原则1091 剂型中含有无活性组分的标示1092 溶出试验方法的发展和验证1101 药用滴管1111 非灭菌药品的微生物特征1111 非灭菌药品的微生物特征检查：药用原料和药物制剂的判定标准1112 非灭菌药品中的水活性测定，即在同一温度时，药品中水的蒸气压与纯水蒸气压之比，它等于药品在密闭系统中产生相对湿度的1%1116 清洁室和其他受控环境的微生物评价1117 微生物实验室的质量规范（GLP）1118 监控装置：时间、温度、湿度1119 近红外分光光度法1120 拉曼（Raman）分光光度法1121 药品命名法1136 药品包装：应用单元1146 口服固体药分装在单疗程剂量容器中的检查方法1150 药物剂型的稳定性1151 药物剂型1160 处方调配的药学计算1171 原料药的位相溶解度分析1174 粉末流动性测定1176 处方天平和容量装置1177 包装质量规范1178 分装质量规范1181 扫描电子显微镜1191 调剂工作中的药品稳定性保持1196 药典协调（指欧洲药典、美国药典、日本药局方三方机构讨论协调的原则和方法）1207 灭菌产品包装：完整性评价1208 灭菌试验：隔离系统的验证1209 灭菌：化学和物理化学的指示剂与积分仪1211 药典收载品种的灭菌和灭菌保证1216 片剂脆性检查1221 茶匙（家用标准为5 ml，可作为病人口服液体药物的量具，误差应小于10%）1222 药品灭菌终点的放行参数1223 微生物替代方法的验证1225 药典方法的验证1227 在抗菌效力、微生物限度、灭菌等试验中，微生物的恢复验证1230 血液透析用水1231 药用水的制备和要求1241 在制药系统中，水—固体的相互作用1251 用分析天平称量的要求1265 书写药物处方的指导原则三、饮食增补剂2021 营养和饮食增补剂的微生物计数试验2022 营养和饮食增补剂中不允许存在的微生物（如金葡菌、沙门氏菌、大肠杆菌、梭状芽胞杆菌属）检查法2023 非灭菌的营养和饮食增补剂中的微生物特征2030 植物来源物品的增补资料2040 饮食增补剂的崩解和溶出检查2091 饮食增补剂的重（装）量差异检查2750 饮食增补剂的生产条件与质量要求（与药品有别）。

USP 34 621 色谱法中文译稿

USP 34 621 色谱法中文译稿美国药典会议官方制订通则: <621> 色谱法页码:1/13<621>色谱法介绍色谱分离技术是通过样品组分在固定相和流动相两相中的分布差异进行分离的技术。

其中固定相可以是固体、有固相支持的液体或凝胶。

固定相可以填充于柱、分散成层、分布为膜或者应用于其他技术中。

流动相可以为气态、液态或超临界流体。

分离可以基于吸附性、质量分布(分配)或离子交换，也可以基于分子物理化学性质的差异，如大小、质量和体积。

本章节包括了基本步骤、定义和对一般参数的计算并描述了对于系统适应性的基本要求。

在USP中应用于定量和定性分析的色谱方法类型有柱色谱法、气象色谱法、纸色谱法、薄层色谱法(包括高效薄层色谱)和加压液相色谱法(一般称作高压或高效液相色谱)。

基本步骤本部分描述了使用某种色谱方法的基本步骤。

除另有各论规定外，以下色谱分离方法的步骤将会被遵循。

纸色谱法固定相:固定相为一张适当质地和厚度的纸。

色谱图的形成过程可以是上行的，这样溶剂被毛细管作用力支撑着沿着纸向上，这个过程也可以是下行的，在此情况下溶剂流动也受到重力的影响。

与溶剂流动有关的纸张纹理定向应该在一系列色谱图中保持恒定。

(纤维方向通常由制造商在色谱纸的包装上标出。

) 仪器:纸色谱法的必备仪器包括装有添加溶剂的入口的气密室和短于该室内部高度5cm的耐腐蚀材料支架。

该支架作为用于溶剂槽以及用于抗虹吸棒的支撑，这些抗虹吸棒依次撑起色谱纸。

气密室的底部以规定的容积系统或流动相覆盖。

使用以规定溶剂系统润湿的纸张衬托于气密室的内壁，以增加气密室的溶剂蒸汽饱和度。

斑点:将待分析的一个或多个物质溶解于适当溶剂中。

以微量吸管吸取适当体积的溶液，其中通常含有1-20µg该化合物，点样为6-10mm大小斑点且斑点间的间隔不小于3cm。

下行色谱法步骤1. 带斑点的色谱纸以抗虹吸棒悬挂在气密室内，该棒将该色谱纸的上端固定在溶剂槽中。

药典液相色谱条件调整范围举例说明

各国药典液相色谱条件调整范围在采用药典方法对药品进行检测时，难免需要对药典中的方法进行调整，以达到更好的分离检测效果。

好多朋友并不能准确清晰了解能不能调、怎么调？下面就这个问题进行了说明，主要是以药典的液相色谱条件中流动相调整为例，其他部分如色谱柱、温度、进样量等可自行参考药典相关部分。

首先，能不能对药典液相色谱条件进行调整？答案当然是可以，但是要遵循一定的调整要求，超出该范围的就需要进行再验证。

调整范围是多少？不同的药典有不同的要求，下面以中国药典2015版、欧洲药典8.0版和美国药典USP36版为例进行说明。

1. 中国药典中国药典-0521高效液相法对此进行了说明，调整流动相组分比例时：当小比例组分的百分比例X小于等于33%时，允许改变范围为0.7 X～1.3 X ;当X大于33%时，允许改变范围为X-10%～X + 10%。

都是中文，这里就不在举例说明了，见下面附图。

2. 欧洲药典欧洲药典-2.2.46 Chromatographic separation techniques对此进行了说明，以等度洗脱为例，调整流动相组分比例时：小比例组分的调整范围是“相对30%或绝对2%”，取其大。

举个栗子：对于一个10%的组分，相对30%的调整范围是7%-13%，绝对2%的调整范围是8%-12%，因此适用相对30%的调整范围。

对于一个5%的组分，相对30%的调整范围是3.5%-6.5%，绝对2%的调整范围是3%-7%，因此适用绝对2%的调整范围。

3. 美国药典美国药典-<621> Chromatography部分对此进行了说明，调整流动相组分比例时：小比例组分（≤50%）的调整范围是“相对30%或绝对10%”，就不再举栗进行细节说明了，感兴趣的朋友可以参阅以下部分：。

美国药典USP3NF26色谱621(DOC74页).doc

美国药典USP3NF26色谱621（DOC74页）621CHROMATOGRAPHY色谱法INTRODUCTION介绍This chapter defines the terms and procedures used in chromatography and provides general information. Specific requirements for chromatographic procedures for drug substances and dosage forms, including adsorbent and developing solvents, are given in the individual monographs.此章节定义了色谱法中用到的术语和步骤，并提供了通用信息。

对于原料药和成药的色谱步骤的具体要求，包括吸附剂和展开溶剂，在具体各论中给出。