欧洲药典附录
欧盟GMP(EUGMP)中文版欧洲药品生产和质量管理规范附录1,无菌药品生产
欧盟GMP(EUGMP)中文版欧洲药品生产和质量管理规范附录1,无菌药品生产盟欧盟 GMP cfu/4 小时 cfu/碟5 指手套cfu/手套A <1 <1 <1 <1B 10 5 5 5C 100 50 25 －D 200 100 50 －注：（a）表中各数值均为平均值。
（b）单个沉降碟的暴露时间可以少于 4 小时。
6.应当对微粒和微生物监控制定适当的警戒和纠偏标准。
操作规程中应详细说明结果超标时应采取的纠偏措施。
隔离技术 7.采用能最大限度降地低生产区人员影响的隔离技术，可大大降低无菌生产中环境对产品微生物污染的风险。
隔离操作台和传递装置的设计可以有多种形式。
隔离操作台及其所处环境的设计，应能保证相应区域空气的质量达到设定标准。
隔离操作台所采用的材料在某种程度上易被穿剌或易产生渗漏。
传输装置可设计成单门的、双门的，甚至可以是同灭菌设备相连的全密封系统。
将物品放入隔离操作台或从中取出属污染风险最为严重的操作过程。
尽管人们认为这类隔离操作器的工作区内不一定要有层流，但是，隔离系统通常是用于进行高污染风险操作的场所。
隔离操作台所处环境的级别取决于它们的设计及其应用。
无菌操作的隔离操作台所处环境的级别应予控制，至少为 D 级。
8.隔离操作台只有经过适当的验证之后方可投入使用。
验证时应当考虑到隔离技术的所有关键性因素，例如，隔离系统内部和外部（所处环境）的空气质量、隔离操作台的消毒、传递操作以及隔离系统的完好性。
9.隔离操作器和隔离用袖管/手套系统应进行常规监测，这包括经常进行必要的检漏试验。
吹气/灌装/密封技术 10.吹气/灌装/密封系统是一套专用机械设备，连续操作，从一个热塑性颗粒吹制成容器至灌装和密封，整个过程由一台全自动机器完成。
用于无菌生产的吹气/灌装/密封设备本身装有 A 级空气风淋装置，在操作人员按A/B 级区要求着装的条件下，该设备可以安装在洁净度至少为C 级的环境中。
eugmp附录1解读 -回复
eugmp附录1解读-回复关于eugmp附录1的解读。
EUGMP附录1是欧洲药典对于药品生产质量管理的指导性文件，其主要内容包括制造药品所需的基本原则、责任的分工、环境设施、原料质量控制、生产过程控制、产品质量检验等方面的要求。
本文将一步一步回答关于EUGMP附录1的解读，探讨其对于药品质量管理的重要性和影响。
首先，我们将解读EUGMP附录1中关于制造药品的基本原则。
根据该附录，制药企业应当确保药品的质量和安全性。
为了达到这个目的，企业需要建立一个有效的质量管理体系并贯彻执行，包括明确的责任分工、合适的员工培训和适当的设备设施等。
这些基本原则为制药企业提供了制造高质量药品的基础。
然后，我们将分析EUGMP附录1中关于责任的分工。
根据该附录，生产药品的责任应当明确划分，确保每个工作岗位的职责和权力清晰，以防止责任不明确和任务重叠的情况发生。
此外，附录1还强调质量管理部门的重要性，并鼓励企业建立一个专门的质量管理小组来监督和评估质量管理体系的实施情况。
接着，我们将讨论EUGMP附录1中关于环境设施的要求。
根据该附录，制药企业应当设立适当的生产场所，并保持良好的环境条件。
这包括合适的温度、湿度和洁净度等因素的控制，以确保药品生产过程的稳定性和一致性。
此外，附录1还要求企业定期检查和验证环境设施，确保其持续符合要求。
然后，我们将探讨EUGMP附录1中关于原料质量控制的内容。
根据该附录，制药企业应当确保所使用的原料符合质量要求，并建立相应的供应商评估和选择机制。
此外，附录1还要求企业对原料进行适当的质量检查和检验，并确保其符合药典要求。
这种原料质量控制的要求有助于提高药品的质量和安全性。
最后，我们将研究EUGMP附录1中关于生产过程控制和产品质量检验的要求。
根据该附录，生产过程应当被有效控制和监督，以确保药品的一致性和稳定性。
附录1还要求企业建立适当的质量控制系统，并对每个生产批次进行质量检验和分析，以确保产品符合规定的质量标准。
欧洲药典附录19
When you decide to stick to one thing, the whole world will make way for you.悉心整理祝您一臂之力（页眉可删）关于药品销售年终工作总结四篇药品销售年终工作总结篇1药店的工作结束了，在一年的工作中，我们顺利的完成了工作。
虽然有着很多的不足之处，但是药店还是顺利的度过的危机，迎来了新的一年。
在这一年中，发生了很多的事情，但是总体来说还是很好的。
回顾过去的一年，现将工作总结如下：一、存在的问题1.以前患者从医院看完病拿着处方去我们店买药，可现在去医院挂号的同时发一张卡，医生开药时直接就打到卡里，患者根本就不知道医生开的是什么药。
所以，之前跑方的药卖的特别好，虽然毛利不高但是有客观的销售额。
可现在一个月也买不了几盒了。
2.顾客经常反映药品价格贵，有的顾客就到别的药店去买了。
还有缺货断货的情况。
二、销售业绩分析（1）20__年与20__年对比；年份成药销售毛利器械毛利保健品毛利20__年 1538085 401540 136933.8 33042 124808 2306620__年 1465571.22 430401.01 117034 23728 88202 16661 （2）20__年完成情况：20__年元月—11月销售额1670807.22。
完成全年的80%。
在上面的两年间对比和20__年完成情况来看，20__年的销售情况并不理想。
三、准备改进的措施1、药品销售技巧：当顾客走进药店，首先要根据对症买药的原则，往往要对营业员提出有关药品的种种疑问，这就要求营业员具备一定的医药知识，对顾客热情作出对症释疑。
只有当顾客的疑虑全部消除以后，明白药物特性和药效，以及有关剂量和服用方法后，顾客方会由购药欲望，转向为购药行为。
顾客购药的心愿是药到病除，而营业员也希望做到这一点，说明药效确实好，这样就能留住一定的顾客群。
2、微笑服务：微笑是一种抚慰，它可以对他人“一笑值千金”。
欧洲药典8.0版附录2.9.40具体内容
欧洲药典8.0版附录2.9.40是一项具有重要意义的内容，它包含了关于卫生产品和医药制剂的质量要求和标准。
在这篇文章中，我们将深入探讨这一主题，从基础概念到具体内容，帮助你更好地理解欧洲药典8.0版附录2.9.40。
1. 了解欧洲药典8.0版附录2.9.40欧洲药典是欧洲药典委员会制定的标准规范，旨在保障卫生产品和医药制剂的质量、安全和有效性。
附录2.9.40则是其中的重要内容之一，它详细规定了一系列的质量要求，涵盖了原材料的选择、生产过程的控制、成品的质量检验等方方面面。
这些要求旨在确保药品的质量稳定、安全性高、有效性强。
2. 欧洲药典8.0版附录2.9.40的具体内容欧洲药典8.0版附录2.9.40的具体内容主要包括以下几个方面：- 原材料的要求：包括对原材料的来源、制备、存储和使用的规定，确保原材料的质量稳定和可追溯性。
- 生产过程的控制：包括药品的生产工艺、设备、人员培训等方面的要求，确保生产过程稳定可控、符合GMP要求。
- 药品的质量检验：包括对成品药品的各项质量指标和检测方法的规定，确保药品符合质量标准。
3. 个人观点和理解欧洲药典8.0版附录2.9.40的具体内容凸显了对药品质量和安全的高标准要求，这种规范的制定对保障患者用药安全、促进药品质量提升有着重要的意义。
而且，这种规范也对制药企业的生产经营提出了更高的要求，能够推动行业向着更加规范、科学的方向发展。
总结回顾通过本文的阐述，相信你对欧洲药典8.0版附录2.9.40有了更深入的了解。
这一规范的制定和实施，促进了药品质量的提升、促进了医药行业的良性发展，对患者和企业来说都具有重要意义。
希望你能在日常工作和学习中，更加关注和重视这一规范，促进药品质量和安全的保障。
4. 药品质量和安全的重要性药品质量和安全对于患者的健康和生命安全具有重要的意义。
优质的药品能够有效治疗疾病，保障患者的健康。
然而，如果药品质量不达标或者存在安全隐患，可能会导致患者用药失败或者出现严重的副作用，危及患者的生命安全。
eugmp附录1解读 -回复
eugmp附录1解读-回复“eugmp附录1解读”首先，需要明确eugmp是什么意思。
eugmp是欧洲药典协会（European Union Good Manufacturing Practices）的缩写，该协会制定了一系列药品生产管理的规范和指南，旨在确保药品的质量和安全性。
而“eugmp 附录1”则是eugmp的第一个附录，其中详细陈述了药品生产过程中的规定和要求。
eugmp附录1主要涵盖了药品生产过程中的设备、人员、文档等各个环节的规定。
下面将按照这些环节一步一步进行解读和回答。
1. 设备：根据eugmp附录1的规定，药品生产过程中所使用的设备必须符合一定的标准，例如必须具备适当的清洁性能、可靠性能和操作性能等。
此外，还要求对设备进行定期的维护和保养，并保证其符合相应的验证要求。
同时，还要求设备的使用必须经过适当的培训和授权，并进行记录。
2. 人员：eugmp附录1对药品生产过程中的人员要求也十分严格。
首先，要求药品生产厂家必须拥有足够的员工，以保证药品生产过程的顺利进行。
其次，要求严格培训和授权所有参与药品生产的人员，确保其具备足够的专业知识和技能。
此外，还要求人员要定期接受必要的培训和教育，以保证其在生产过程中的操作符合相应的标准。
3. 文档：eugmp附录1还对药品生产过程中的文档管理提出了要求。
具体来说，要求药品生产厂家必须确保所有的生产文档都要进行准确和完整的记录，包括原料的采购记录、生产过程中的记录以及产品的出货记录等。
此外，还要求对这些记录进行适当的存档和管理，以供后续的审查和追溯。
综上所述，eugmp附录1对药品生产过程中的设备、人员和文档等环节都提出了明确的要求。
这些要求旨在确保药品的质量和安全性，防止药品生产过程中出现的差错和问题。
只有严格遵守eugmp附录1的规定，药品生产厂家才能生产出高质量、安全可靠的药品，以满足患者和社会的需求。
然而，光有规定还不够，必须要有监督和执行的机制来确保这些规定得到遵守。
（完整版）欧盟GMP附录
（完整版）欧盟GMP附录欧洲共同体：European Communities (EC)。
欧洲联盟：European Union (EU)，简称欧盟。
⼈⽤药品注册技术标准国际协调会：ICH欧盟GMP附录1⽆菌药品的⽣产注：冻⼲瓶轧盖的条款⾃2010年3⽉1⽇开始实施。
原则为降低微⽣物、微粒和热原污染的风险，⽆菌药品的⽣产应有各种特殊要求。
这在很⼤程度上取决于⽣产⼈员的技能、所接受的培训及其⼯作态度。
质量保证极为重要，⽆菌药品的⽣产必须严格按照精⼼制订并经验证的⽅法和规程进⾏。
产品的⽆菌或其它质量特性绝不能仅依赖于任何形式的最终操作或成品检验。
注：本指南没有对微粒、浮游菌和表⾯微⽣物等测试⽅法详细进⾏阐述，可参阅欧洲标准或国际标准（CEN/ISO）及药典资料。
总则1.⽆菌药品的⽣产必须在洁净区内进⾏，⼈员和（或）设备以及物料必须通过缓冲进⼊洁净区。
洁净区应当保持适当的洁净度，洁净区的送风须经具有⼀定过滤效率过滤器的过滤。
2.原料配制、产品加⼯和灌装等不同操作必须在洁净去内彼此分开的单独区域内进⾏。
⽣产⼯艺可分为两类：⼀类是最终灭菌⼯艺；第⼆类是部分或全部⼯序为⽆菌操作的⼯艺。
3.应按所需环境的特点确定⽆菌产品的洁净级别。
每⼀步⽣产操作都应达到适当的动态洁净度，以尽可能降低产品（或原料）被微粒或微⽣物污染。
洁净区的设计必须符合相应的“静态”标准，以达到“动态”的洁净要求。
“静态”是指安装已经完成并已运⾏，但没有操作⼈员在场的状态。
“动态”是指⽣产设施按预定的⼯艺模式运⾏并有规定数量的操作⼈员进⾏现场操作的状态。
应确定每⼀洁净室或每组洁净间的“动态”及“静态”标准。
⽆菌药品⽣产所需的洁净区⼀般可分为4个级别：A级：⾼风险操作区，如：灌装区，放置胶塞桶、敞⼝安瓿瓶、敞⼝西林瓶的区域及⽆菌装配/连接操作的区域。
通常⽤单向流操作台/罩来维护该区的环境状态。
单向流系统在其⼯作区域必须均匀送风，风速为0.36-0.54m/s（指导值）。
欧洲药典7.0附录炽灼残渣 熔点 干燥失重 重金属
熔点：毛细管法测定的熔点是由原来的固体颗粒紧列物质转变为液态时的温度。
专注规定，该装置和方法，用于测定其他因素，如液面凹陷或熔化范围，来描述物质的熔化过程。
装置。
该装置由：-一个合适的玻璃容器含有液体浴（例如，水，液体石蜡或硅油）和安装一个合适的加热装置，-一个合适的手段，搅拌，保证了温度的均匀性的浴室内，-一个合适的温度计毕业不超过0.5摄氏°间隔设有浸泡标记。
一系列的温度不超过100摄氏°，-无碱硬玻璃毛细管内径0.9毫米到1.1毫米与0.10毫米至0.15毫米，壁厚和一端封闭除非另有规定，干燥的细粉状物质在真空和无水硅胶为24小时介绍了足够数量的毛细管管给紧凑型柱4毫米到6毫米的高度。
提高浴的温度约10摄氏°以下的假定的熔点和调整加热速度约1°℃/分钟。
当温度为5℃以下的假定°熔点，正确地介绍了毛细管管插入仪器。
对上述设备，使毛细管管，封闭端附近的中心温度计的灯泡，浸泡标记，是一级液体表面。
记录温度在过去的粒子进入液相校准装置。
该仪器可以校准使用熔点参考物质如世界卫生组织或其他适当的物质。
干燥失重干燥失重质量损失表示质量分数的方法。
将一定量的待测物质在干燥至恒重的称量瓶中检测。
干燥待测物质至恒重或按下列步骤干燥，浮动范围为±2°C。
A, 在干燥器中：常温常压下，以五氧化二磷干燥。
B，真空干燥：室温下，在压强为1.5千帕～2.5千帕，放置五氧化二磷的真空干燥箱内干燥。
C，要求温度范围内真空干燥：在专论规定的温度范围内，压强为1.5千帕～2.5千帕，放置五氧化二磷的真空干燥箱内干燥。
D，在要求温度范围内的干燥箱内干燥：在专论规定的温度范围内干燥E，高真空干燥：在专论规定的温度范围内，压力不超过0.1千帕，放置五氧化二磷的真空干燥箱内干燥。
如有其它要求的条件，根据专论中的具体规定操作。
干燥失重可按下列公式计算：B-C干燥失重（%）= × 100B-AA 称量瓶重量（g）B 干燥前称量瓶与样品的重量（g）C 干燥后称量瓶与样品的重量（g）重金属方法A供试溶液：12ml待测水溶液，2ml pH为3.5的缓冲溶液，混合后加1.2ml 的硫代乙酰胺试液，立即混合。
欧洲药典中文翻译
附录1溶液的澄清度在内径15～25mm，平底，无色、透明、中性玻璃管中，加入等量的供试溶液与浊度标准液，使液位的深度都为40mm，按如下所述方法进行比较。
浊度标准液制备5分钟后，以色散自然光照射浊度标准溶液和供试溶液，在黑色背景下从垂直方向观察、比较澄清度或浑浊程度。
色散自然光必须较容易区分浊度标准溶液Ⅰ与水，浊度标准溶液Ⅱ与浊度标准溶液Ⅰ。
如果供试溶液的澄清、透明程度与水相同，或者与所用溶剂相同，或者其澄清度不超过Ⅰ号浊度标准溶液，那么可判定该溶液为澄清。
试剂：硫酸肼溶液：取硫酸肼溶于水，加水稀释至，静置4～6小时。
乌洛托品（六亚甲基四胺）溶液：在100ml容量平中，以水溶解乌洛托品。
浊度标准贮备液：在存放乌洛托品溶液的100ml容量瓶中，加的硫酸肼溶液。
混合，静置24小时，贮存在无表面要求的玻璃容器中，可在2个月内使用。
该浊度液不得黏附玻璃，用前必须充分摇匀。
浊度标准原液：取浊度标准贮备液15ml，加水稀释、定容至1000ml。
该液临用前制备，至多保存24小时。
浊度标准液：由浊度标准原液与水按表1-1配制,即得。
本液应临用前配制。
表1-1附录2 溶液颜色检查按本药典规定，用下面两种方法之一可以检出溶液在棕色-黄色-红色范围内的颜色。
如果溶液A的外观与水或所用溶剂相同，或者颜色浅于标准比色液B9，则可判定溶液A为无色。
方法I用外径为12mm的无色、透明中性玻璃管取2ml的供试溶液，与相同玻璃管中的2ml的水，或2ml本文所规定的标准比色液（见标准比色液表）进行比较。
在散射自然光，白色的背景下，水平观察比较颜色。
方法Ⅱ用同样平底、内径为15～25mm的无色透明中性玻璃管，液位的深度为40mm，将供试溶液与水或溶剂或本文中规定的标准比色液（见标准比色液表）对比。
在散射自然光，白色的背景下，垂直地观察比较颜色。
贮备液黄色液称取46克氯化铁，加大约900ml盐酸溶液（25ml浓盐酸和975ml水混和）溶解，继续添加，并定容。
(完整版)欧盟GMP附录
欧洲共同体：European Communities (EC)。
欧洲联盟：European Union (EU)，简称欧盟。
人用药品注册技术标准国际协调会：ICH欧盟GMP附录1无菌药品的生产注：冻干瓶轧盖的条款自2010年3月1日开始实施。
原则为降低微生物、微粒和热原污染的风险，无菌药品的生产应有各种特殊要求。
这在很大程度上取决于生产人员的技能、所接受的培训及其工作态度。
质量保证极为重要，无菌药品的生产必须严格按照精心制订并经验证的方法和规程进行。
产品的无菌或其它质量特性绝不能仅依赖于任何形式的最终操作或成品检验。
注：本指南没有对微粒、浮游菌和表面微生物等测试方法详细进行阐述，可参阅欧洲标准或国际标准（CEN/ISO）及药典资料。
总则1.无菌药品的生产必须在洁净区内进行，人员和（或）设备以及物料必须通过缓冲进入洁净区。
洁净区应当保持适当的洁净度，洁净区的送风须经具有一定过滤效率过滤器的过滤。
2.原料配制、产品加工和灌装等不同操作必须在洁净去内彼此分开的单独区域内进行。
生产工艺可分为两类：一类是最终灭菌工艺；第二类是部分或全部工序为无菌操作的工艺。
3.应按所需环境的特点确定无菌产品的洁净级别。
每一步生产操作都应达到适当的动态洁净度，以尽可能降低产品（或原料）被微粒或微生物污染。
洁净区的设计必须符合相应的“静态”标准，以达到“动态”的洁净要求。
“静态”是指安装已经完成并已运行，但没有操作人员在场的状态。
“动态”是指生产设施按预定的工艺模式运行并有规定数量的操作人员进行现场操作的状态。
应确定每一洁净室或每组洁净间的“动态”及“静态”标准。
无菌药品生产所需的洁净区一般可分为4个级别：A级：高风险操作区，如：灌装区，放置胶塞桶、敞口安瓿瓶、敞口西林瓶的区域及无菌装配/连接操作的区域。
通常用单向流操作台/罩来维护该区的环境状态。
单向流系统在其工作区域必须均匀送风，风速为0.36-0.54m/s（指导值）。
欧洲药典附录2612非无菌产品的微生物限度检查之一有活力的需氧菌总数的计数
准备一．系列（至少三个）连续的ｌ：１０稀释度的 样品，每一个连续稀释度均ｌ克或１毫升接种到装 有９毫升适合的液体培养基（ｉｎ肉汤培养基Ａ）的试
类别】：正常的结果。９５跖的情况下得到此种结
褒２ ６．１２一ｌ——细茵的最大可能数评价
０ １克
阳性管数目 ０ ０１克
０．００１克
每一稀释度各三营
每克样品最 大可能数
类别
２
９５蟛置信区间
１ ２
２
２ ２
２
２
３
｝０
ｌ
３
ｌ
２
２
Ｚ
３
３ ３
１ｌ
９
１
１４
１５
１
２０
２ｌ ２３
ｌ
３８
ｌ
７５
９３
１
ｌ ５０
２
２ｉ０
２４０
Ｐａｎ Ｈａｉｘｉａ（Ｃａｎｇｚｆｕ＊Ｉｎｓｔｉｔｕｔｅ向Ｄｒｕｇ Ｃ，：，ｍｒｏｌ，ＣａｎｇｚｈｏｕｔＨｅｂｅｉ ｐｒｏｖｉｎｃｅ ０６１００１）
《中国药典｝２０００年版二部详细规定了消旋山莨 菪碱片的含量均匀度和含量测定方法。在实际检验工 作中笔者发现，本标准不太严密，提出两点以供商榷：
１．含量均匀度检查项下“加甲基红一溴甲酚绿 （１：３）混合指示液５滴”，但甲基红溶液与漠甲酚绿 溶液的浓度并未指明。若按照《中国药典））２０００年版 二部附录ｘＶ Ｅ指示剂与指示液中“甲基红一溴甲 酚绿混合指示液”的方法“取０．１％甲基红的乙醇溶 液２０ｍｌ，加０．２％溴甲酚绿的乙醇溶液３０ｍｌ。摇匀， 即得。”配制，二者的混合比例为２：３，与标准中的１ ：３不符，且二者的浓度与含量测定项也不一致。
欧洲药典附录3.1.3.大全
3.1.3. 聚烯烃定义聚烯烃是通过乙烯或丙烯的聚合而成，或是通过这些不超过25%的高同系物的物质或羧酸或酯的共聚作用获得。
某些材料可能是聚烯烃的混合物。
成品添加一定数量的添加剂到聚合物中是为了优化它们的化学性质，物理性质和机械性能，为了使它们适用于预定用途。
所有的这些添加剂都是选自附件列表，并指出了每一种产品中的最大允许含量。
产品中最多包含有三种抗氧化剂，一种或几种润滑剂或抗粘连剂以及当材料必须提供光照保护时，还要添加二氧化钛作为遮光剂。
–二叔丁基对甲酚（增塑剂07）：限量：0.125%–四钛季戊四醇松香酸酯[3-(3,5-二叔丁基-4-羟苯基)丙酸酯]（增塑剂09）：限量：0.3% –1,3,5-三羟甲基氨基甲烷(3,5-二叔丁基-4-邻羟苄基 )- 三嗪-2,4,6(1H,3H,5H)-三酮, (增塑剂 13): 限量： 0.3%–二乙烯[3,3-二[3-(1,1-dimethylethyl)-4-羟苯基]丁酸甲酯] (增塑剂08)：限量：0.3% –二（十八烷基）二硫化物（增塑剂15）限量：0.3%4,4′,4″-(2,4,6-三甲基苯-1,3,5-triyltrismethylene)–三羟甲基氨基甲烷[2,6-二(1,1-dimethylethyl)苯酚]（增塑剂10）限量：0.3%2,2′-二(octadecyloxy)-5,5′-spirobi[1,3,2-dioxaphosphinane](增塑剂 14): 限量：0.3 %;–didodecyl 3,3′-硫代二丙酸（增塑剂16): 限量： 0.3 %;–dioctadecyl3,3′-硫代二丙酸(增塑剂 17): 限量：0.3 %;–三羟甲基氨基甲烷[2,4-二(1,1-dimethylethyl)苯基] 亚磷酸盐 (增塑剂 12): 限量：0.3 %;–增塑剂 18: 限量： 0.1%;–琥珀酸二甲酯和 (4-hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)乙醇的共聚物 (增塑剂 22): 限量：0.3%上面列出的抗氧化添加剂总含量不超过0.3%。
欧洲药典附录中文翻译
附录1溶液的澄清度在内径15～25mm，平底，无色、透明、中性玻璃管中，加入等量的供试溶液与浊度标准液，使液位的深度都为40mm，按如下所述方法进行比较。
浊度标准液制备5分钟后，以色散自然光照射浊度标准溶液和供试溶液，在黑色背景下从垂直方向观察、比较澄清度或浑浊程度。
色散自然光必须较容易区分浊度标准溶液Ⅰ与水，浊度标准溶液Ⅱ与浊度标准溶液Ⅰ。
如果供试溶液的澄清、透明程度与水相同，或者与所用溶剂相同，或者其澄清度不超过Ⅰ号浊度标准溶液，那么可判定该溶液为澄清。
试剂：硫酸肼溶液：取1.0g硫酸肼溶于水，加水稀释至100.0ml，静臵4～6小时。
乌洛托品（六亚甲基四胺）溶液：在100ml容量平中，以25.0ml水溶解2.5g 乌洛托品。
浊度标准贮备液：在存放乌洛托品溶液的100ml容量瓶中，加25.0ml的硫酸肼溶液。
混合，静臵24小时，贮存在无表面要求的玻璃容器中，可在2个月内使用。
该浊度液不得黏附玻璃，用前必须充分摇匀。
浊度标准原液：取浊度标准贮备液15ml，加水稀释、定容至1000ml。
该液临用前制备，至多保存24小时。
浊度标准液：由浊度标准原液与水按表1-1配制,即得。
本液应临用前配制。
表1-1附录2溶液颜色检查按本药典规定，用下面两种方法之一可以检出溶液在棕色-黄色-红色范围内的颜色。
如果溶液A的外观与水或所用溶剂相同，或者颜色浅于标准比色液B9，则可判定溶液A为无色。
方法I用外径为12mm的无色、透明中性玻璃管取2ml的供试溶液，与相同玻璃管中的2ml的水，或2ml本文所规定的标准比色液（见标准比色液表）进行比较。
在散射自然光，白色的背景下，水平观察比较颜色。
方法Ⅱ用同样平底、内径为15～25mm的无色透明中性玻璃管，液位的深度为40mm，将供试溶液与水或溶剂或本文中规定的标准比色液（见标准比色液表）对比。
在散射自然光，白色的背景下，垂直地观察比较颜色。
贮备液黄色液称取46克氯化铁，加大约900ml盐酸溶液（25ml浓盐酸和975ml水混和）溶解，继续添加，并定容1000.0ml。
欧盟药品GMP附录2人用生物制品英文原版
欧盟药品GMP附录2人用生物制品英文原版ANNEX 2MANUFACTURE OF BIOLOGICAL MEDICINAL PRODUCTS FOR HUMAN USEScopeThe methods employed in the manufacture of biological medicinal products are a critical factor in shaping the appropriate regulatory control. Biological medicinal products can be defined therefore largely by reference to their method of manufacture. Biological medicinal products prepared by the following methods of manufacture will fall under the scope of this annex (1).Biological medicinal products manufactured by these methods include: vaccines, immunosera, antigens, hormones, cytokines, enzymes and other products of fermentation (including monoclonal antibodies and products derived from r-DNA).a) Microbial cultures, excluding those resulting from r-DNA techniques;b) Microbial and cell cultures, including those resulting from recombinant DNA or hybridomatechniques;c) Extraction from biological tissuesd) Propagation of live agents in embryos or animals(Not all of the aspects of this annex may necessarily apply to products in category a).NoteIn drawing up this guidance, due consideration has beengiven to the general requirements for manufacturing establishments and control laboratories proposed by the WHO.The present guidance does not lay down detailed requirements for specific classes of biological products, and attention is therefore directed to other guidelines issued by the Committee for Proprietary Medicinal Products (CPMP), for example the note for guidance on monoclonal antibodies and the note for guidance on products of recombinant DNA technology (“The rules governing medicinal product in the European Community”, Volume 3).PrincipleThe manufacture of biological medicinal products involves certain specific considerations arising from the nature of the products and the processes. The way in which biological medicinal products are produced, controlled and administered make some particular precautions necessary.Unlike conventional medicinal products, which are reproduced using chemical and physical techniques capable of a high degree of consistency, the production of biological medicinal products involves biological processes and materials, such as cultivation of cells or extraction of material from living organisms. These biological processes may display inherent variability, so that the range and nature of by-products are variable. Moreover, the materials used in these cultivation processes provide good substrates for growth of microbial contaminants.Control of biological medicinal products usually involves biological analytical techniques which have a greater variability than physico-chemical determinations. In-process controls therefore take on a great importance in the manufacture ofbiological medicinal products.(1) Biological medicinal products manufactured by these methods include: vaccines, immunosera, antigens, hormones, cytokines, enzymes and other products of fermentation (including monoclonal antibodies and products derived from r-DNA).Personnel1. All personnel (including those concerned with cleaning, maintenance or quality control)employed in areas where biological medicinal products are manufactured should receive additional training specific to the products manufactured and to their work. Personnel should be given relevant information and training in hygiene and microbiology.2. Persons responsible for production and quality control should have an adequate background inrelevant scientific disciplines, such as bacteriology, biology, biometry, chemistry, medicine, pharmacy, pharmacology, virology, immunology and veterinary medicine, together with sufficient practical experience to enable them to exercise their management function for the process concerned.3. The immunological status of personnel may have to be taken into consideration for productsafety. All personnel engaged in production, maintenance, testing and animal care (and inspectors) should be vaccinated where necessary with appropriate specific vaccines and have regular health checks. Apart from the obvious problem of exposure of staff to infectious agents, potent toxins or allergens, it is necessary to avoid the risk of contamination of a productionbatch with infectious agents. Visitors should generally be excluded from production areas.4. Any changes in the immunological status of personnel which could adversely affect the qualityof the product should preclude work in the production area. Production of BCG vaccine and tuberculin products should be restricted to staff who are carefully monitored by regular checks of immunological status or chest X-ray.5. In the course of a working day, personnel should not pass from areas where exposure to liveorganisms or animals is possible to areas where other products or different organisms are handled. If such passage is unavoidable, clearly defined decontamination measures, including change of clothing and shoes and, where necessary, showering should be followed by staff involved in any such production.Premises and equipment6. The degree of environmental control of particulate and microbial contamination of the productionpremises should be adapted to the product and the production step, bearing in mind the level of contamination of the starting materials and the risk to the finished product.7. The risk of cross-contamination between biological medicinal products, especially during thosestages of the manufacturing process in which live organisms are used, may require additional precautions with respect to facilities and equipment, such as the use of dedicated facilities and equipment, production on a campaign basis and the use of closed systems. The nature of the product as well as the equipment used will determine the level of segregation neededto avoid cross-contamination.8. In principle, dedicated facilities should be used for the production of BCG vaccine and for thehandling of live organisms used in production of tuberculin products.9. Dedicated facilities should be used for the handling of Bacillus anthracis, of Clostridiumbotulinum and of Clostridium tetani until the inactivation process is accomplished.10. Production on a campaign basis may be acceptable for other spore forming organisms providedthat the facilities are dedicated to this group of products and not more than one product is processed at any one time.11. Simultaneous production in the same area using closed systems of biofermenters may beacceptable for products such as monoclonal antibodies and products prepared by DNA techniques.12. Processing steps after harvesting may be carried out simultaneously in the same productionarea provided that adequate precautions are taken to prevent cross contamination. For killed vaccines and toxoids, such parallel processing should only be performed after inactivation of the culture or after detoxification.13. Positive pressure areas should be used to process sterile products but negative pressure inspecific areas at point of exposure of pathogens is acceptable for containment reasons.Where negative pressure areas or safety cabinets are used for aseptic processing of pathogens, they should be surrounded by a positive pressure sterile zone.14. Air filtration units should be specific to the processing area concerned and recirculation of airshould not occur from areas handling live pathogenic organisms.15. The layout and design of production areas and equipment should permit effective cleaning anddecontamination (e.g. by fumigation). The adequacy of cleaning and decontamination procedures should be validated.16. Equipment used during handling of live organisms should be designed to maintain cultures in apure state and uncontaminated by external sources during processing.17. Pipework systems, valves and vent filters should be properly designed to facilitate cleaning andsterilisation. The use of ‘clean in place’ and ‘sterilise in place’ systems should be encouraged.Valves on fermentation vessels should be completely steam sterilisable. Air vent filters should be hydrophobic and validated for their scheduled life span.18. Primary containment should be designed and tested to demonstrate freedom from leakage risk.19. Effluents which may contain pathogenic micro-organisms should be effectively decontaminated.20. Due to the variability of biological products or processes, some additives or ingredients have tobe measured or weighed during the production process (e.g. buffers). In these cases, small stocks of these substances may be kept in the production area.Animal quarters and care21. Animals are used for the manufacture of a number ofbiological products, for example poliovaccine (monkeys), snake antivenoms (horses and goats), rabies vaccine (rabbits, mice and hamsters) and serum gonadotropin (horses). In addition, animals may also be used in the quality control of most sera and vaccines, e.g. pertussis vaccine (mice), pyrogenicity (rabbits), BCG vaccine (guinea-pigs).22. General requirements for animal quarters, care and quarantine are laid down in Directive86/609/EEC2. Quarters for animals used in production and control of biological products should be separated from production and control areas. The health status of animals from which some starting materials are derived and of those used for quality control and safety testing should be monitored and recorded. Staff employed in such areas must be provided with special clothing and changing facilities. Where monkeys are used for the production or quality control of biological medicinal products, special consideration is required as laid down in the current WHO Requirements for Biological Substances n° 7.Documentation23. Specifications for biological starting materials may need additional documentation on thesource, origin, method of manufacture and controls applied, particularly microbiological controls.24. Specifications are routinely required for intermediate and bulk biological medicinal products.2Directive 2003/65/EC of the European Parliament and of the Council of 22 July 2003 amending CouncilDirective 86/609/EEC on the approximation of laws, regulations and administrative provisions of the Member States regarding the protection of animals used for experimental andother scientific purposes(OJ L 230, 16.09.2003, p. 32- 33)ProductionStarting materials25. The source, origin and suitability of starting materials should be clearly defined. Where thenecessary tests take a long time, it may be permissible to process starting materials before the results of the tests are available. In such cases, release of a finished product is conditional on satisfactory results of these tests.26. Where sterilisation of starting materials is required, it should be carried out where possible byheat. Where necessary, other appropriate methods may also be used for inactivation of biological materials (e.g. irradiation).Seed lot and cell bank system27. In order to prevent the unwanted drift of properties which might ensue from repeatedsubcultures or multiple generations, the production of biological medicinal products obtained by microbial culture, cell culture or propagation in embryos and animals should be based on a system of master and working seed lots and/or cell banks.28. The number of generations (doublings, passages) between the seed lot or cell bank and thefinished product should be consistent with the marketing authorisation dossier. Scaling up of the process should not change this fundamental relationship.29. Seed lots and cell banks should be adequately characterised and tested for contaminants. Theirsuitability for use should be further demonstrated by the consistency of the characteristics and quality of the successivebatches of product. Seed lots and cell banks should be established, stored and used in such a way as to minimise the risks of contamination or alteration.30. Establishment of the seed lot and cell bank should be performed in a suitably controlledenvironment to protect the seed lot and the cell bank and, if applicable, the personnel handling it. During the establishment of the seed lot and cell bank, no other living or infectious material(e.g. virus, cell lines or cell strains) should be handled simultaneously in the same area or by thesame persons.31. Evidence of the stability and recovery of the seeds and banks should be documented. Storagecontainers should be hermetically sealed, clearly labelled and kept at an appropriate temperature. An inventory should be meticulously kept. Storage temperature should be recorded continuously for freezers and properly monitored for liquid nitrogen. Any deviation from set limits and any corrective action taken should be recorded.32. Only authorised personnel should be allowed to handle the material and this handling should bedone under the supervision of a responsible person. Access to stored material should be controlled. Different seed lots or cell banks should be stored in such a way to avoid confusion or cross-contamination. It is desirable to split the seed lots and cell banks and to store the parts at different locations so as to minimise the risks of total loss.33. All containers of master or working cell banks and seed lots should be treated identically duringstorage. Once removed from storage, the containers shouldnot be returned to the stock.Operating principles34. The growth promoting properties of culture media should be demonstrated.35. Addition of materials or cultures to fermenters and other vessels and the taking of samplesshould be carried out under carefully controlled conditions to ensure that absence of contamination is maintained. Care should be taken to ensure that vessels are correctly connected when addition or sampling take place.36. Centrifugation and blending of products can lead to aerosol formation, and containment of suchactivities to prevent transfer of live micro-organisms is necessary.37. If possible, media should be sterilised in situ. In-line sterilising filters for routine addition ofgases, media, acids or alkalis, defoaming agents etc. to fermenters should be used where possible.38. Careful consideration should be given to the validation of any necessary virus removal orinactivation undertaken (see CPMP notes for guidance).39. In cases where a virus inactivation or removal process is performed during manufacture,measures should be taken to avoid the risk of recontamination of treated products by non-treated products.40. A wide variety of equipment is used for chromatography, and in general such equipment shouldbe dedicated to the purification of one product and should be sterilised or sanitised between batches. The use of the same equipment at different stages of processing should bediscouraged. Acceptance criteria, life span and sanitation or sterilisation method of columns should be defined.Quality control41. In-process controls play a specially important role in ensuring the consistency of the quality ofbiological medicinal products. Those controls which are crucial for quality (e.g. virus removal) but which cannot be carried out on the finished product, should be performed at an appropriate stage of production.42. It may be necessary to retain samples of intermediate products in sufficient quantities and underappropriate storage conditions to allow the repetition or confirmation of a batch control.43. Continuous monitoring of certain production processes is necessary, for example fermentation.Such data should form part of the batch record.44. Where continuous culture is used, special consideration should be given to the quality controlrequirements arising from this type of production method.。
欧洲药典 8.8 附录7 Limit Tests (限量检查法)
(No Ph. Eur. method)Nessler CylindersWhere the use of Nessler cylinders is prescribed in a test of the Pharmacopoeia, Nessler cylinders complying with the following requirements should be used.Nessler cylinders comply with British Standard 612:1966 (Specification for Nessler cylinders). They are of clear glass with a nominal capacity of 50 mL; the overall height is about 15 cm, the external height to the 50-mL mark 11.0 to 12.4 cm, the thickness of the wall 1.0 to 1.5 mm and the thickness of the base 1.0 to 3.0 mm. The external heights to the 50-mL mark of cylinders used for a test must not differ by more than 1 mm.Tubes for Comparative Tests(Ph. Eur. method 2.1.5)Tubes used for comparative tests are matched tubes of colourless glass with a uniform internal diameter. The base is transparent and flat.A column of the liquid is examined down the vertical axis of the tube against a white background, or if necessary, against a black background. The examination is carried out in diffused light.It is assumed that tubes with an internal diameter of 16 mm will be used. Tubes with a larger internal diameter may be used instead but the volume of liquid examined must then be increased so that the depth of liquid in the tubes is not less than where the prescribed volume of liquid and tubes 16 mm in internal diameter are used.Limit Test for Aluminium(Ph. Eur. method 2.4.17)Place the prescribed solution in a separating funnel and shake with 2 quantities, each of 20 mL, and then with one 10 mL quantity of a 5 g/L solution of hydroxyquinoline R in chloroform R . Dilute the combined chloroform solutions to 50.0 mL with chloroform R (test solution).Prepare a standard in the same manner using the prescribed reference solution.Prepare a blank in the same manner using the prescribed blank solution.Measure the intensity of the fluorescence (2.2.21) of the test solution (I 1), of the standard (I 2) and of the blank (I 3) using an excitant beam at 392 nm and a secondary filter with a transmission band centred on 518 nm or a monochromator set to transmit at this wavelength.The fluorescence (I 1-I 3) of the test solution is not greater than that of the standard (I 2-I 3).Limit Test for Ammonium(Ph. Eur. method 2.4.1)Unless otherwise prescribed, use method A.METHOD AIntroduce the prescribed solution into a test-tube or dissolve the prescribed quantity of the substance to be examined in 14 mL of water R in a test-tube. Make the solution alkaline if necessary by the addition of dilute sodium hydroxide solution R , dilute to 15 mL with water R and add 0.3 mL of alkaline potassium tetraiodomercurate solution R . Prepare a standard by mixing 10 mL of ammonium standard solution (1 ppm NH 4) R , 5 mL of water R and 0.3 mL of alkaline potassium tetraiodomercurate solution R . Stopper the test-tubes.After 5 min, any yellow colour in the test solution is not more intense than that in the standard.METHOD BIn a 25 mL jar fitted with a cap, place the prescribed quantity of the finely powdered substance to be examined and dissolve or suspend in 1 mL of water R . Add 0.30 g of heavy magnesium oxide R . Close immediately after placing a piece of silver manganese paper R 5 mm square, wetted with a few drops of water R , under the polyethylene cap. Swirl, avoiding projections of liquid, and allow to stand at 40 °C for 30 min. If the silver manganese paper shows a grey colour, it is not more intense than that of a standard prepared at the same time and in the same manner using the prescribed volume of ammonium standard solution (1 ppm NH 4) R , 1 mL of water R and 0.30 g of heavy magnesium oxide R .Limit Test for Arsenic (Ph. Eur. method 2.4.2)Status: You are viewing the legally effective version.Appendix VII Limit Tests{METHOD AThe apparatus (see Figure 2.4.2.-1) consists of a 100 mL conical flask closed with a ground-glass stopper through which passes a glass tube about200 mm long and of internal diameter 5 mm. The lower part of the tube is drawn to an internal diameter of 1.0 mm, and 15 mm from its tip is a lateral orifice 2 mm to 3 mm in diameter. When the tube is in position in the stopper, the lateral orifice should be at least 3 mm below the lower surface of the stopper. The upper end of the tube has a perfectly flat, ground surface at right angles to the axis of the tube. A second glass tube of the same internal diameter and 30 mm long, with a similar flat ground surface, is placed in contact with the first, and is held in position by two spiral springs. Into the lower tube insert50 mg to 60 mg of lead acetate cotton R, loosely packed, or a small plug of cotton and a rolled piece of lead acetate paper R weighing 50 mg to 60 mg. Between the flat surfaces of the tubes place a disc or a small square of mercuric bromide paper R large enough to cover the orifice of the tube(15 mm × 15 mm).In the conical flask dissolve the prescribed quantity of the substance to be examined in 25 mL of water R, or in the case of a solution adjust the prescribed volume to 25 mL with water R. Add 15 mL of hydrochloric acid R, 0.1 mL of stannous chloride solution R and 5 mL of potassium iodide solution R, allow to stand for 15 min and introduce 5 g of activated zinc R. Assemble the two parts of the apparatus immediately and immerse the flask in a bath of water at a temperature such that a uniform evolution of gas is maintained. Prepare a standard in the same manner, using 1 mL of arsenic standard solution (1 ppm As) R, diluted to 25 mL with water R.After not less than 2 h the stain produced on the mercuric bromide paper in the test is not more intense than that in the standard.METHOD BIntroduce the prescribed quantity of the substance to be examined into a test-tube containing 4 mL of hydrochloric acid R and about 5 mg of potassium iodide R and add 3 mL of hypophosphorous reagent R. Heat the mixture on a water-bath for 15 min, shaking occasionally. Prepare a standard in the same manner, using 0.5 mL of arsenic standard solution (10 ppm As) R.After heating on the water-bath, any colour in the test solution is not more intense than that in the standard.Figure 2.4.2.-1. - Apparatus for limit test A for arsenicDimensions in millimetresLimit Test for Calcium(Ph. Eur. method 2.4.3)All solutions used for this test are prepared with distilled water R.To 0.2 mL of alcoholic calcium standard solution (100 ppm Ca) R add 1 mL of ammonium oxalate solution R. After 1 min add a mixture of 1 mL of dilute acetic acid R and 15 mL of the prescribed solution or of a solution containing the prescribed quantity of the substance to be examined, and shake. Prepare a standard in the same manner using a mixture of 10 mL of aqueous calcium standard solution (10 ppm Ca) R, 1 mL of dilute acetic acid R and 5 mL of distilled water R.After 15 min, any opalescence in the test solution is not more intense than that in the standard.Limit Test for Chlorides(Ph. Eur. method 2.4.4)To 15 mL of the prescribed solution add 1 mL of dilute nitric acid R and pour the mixture as a single addition into a test-tube containing 1 mL of silver nitrate solution R2. Prepare a standard in the same manner using 10 mL of chloride standard solution (5 ppm Cl) R and 5 mL of water R. Examine the tubes laterally against a black background.After standing for 5 min protected from light, any opalescence in the test solution is not more intense than that in the standard.Limit Test for Fluorides(Ph. Eur. method 2.4.5)Introduce into the inner tube of the apparatus (see Figure 2.4.5.-1) the prescribed quantity of the substance to be examined, 0.1 g of acid-washed sand R and 20 mL of a mixture of equal volumes of sulfuric acid R and water R. Heat the jacket containing tetrachloroethane R maintained at its boiling point (146 °C). Heat the steam generator and distil, collecting the distillate in a 100 mL volumetric flask containing 0.3 mL of 0.1 M sodium hydroxide and 0.1 mL of phenolphthalein solution R. Maintain a constant volume (20 mL) in the tube during distillation and ensure that the distillate remains alkaline, adding0.1 M sodium hydroxide if necessary. Dilute the distillate to 100 mL with water R (test solution). Prepare a standard in the same manner by distillation, using 5 mL of fluoride standard solution (10 ppm F) R instead of the substance to be examined. Into two glass-stoppered cylinders introduce 20 mL of the test solution and 20 mL of the standard and 5 mL of aminomethylalizarindiacetic acid reagent R.After 20 min, any blue colour in the test solution (originally red) is not more intense than that in the standard.Figure 2.4.5.-1. – Apparatus for limit test for fluoridesDimensions in millimetresLimit Test for Heavy Metals(Ph. Eur. method 2.4.8)The methods described below require the use of thioacetamide reagent R. As an alternative, sodium sulfide solution R1 (0.1 mL) is usually suitable. Since tests prescribed in monographs have been developed using thioacetamide reagent R, if sodium sulfide solution R1 is used instead, it is necessary to include also for methods A, B and H a monitor solution, prepared from the quantity of the substance to be examined prescribed for the test, to which has been added the volume of lead standard solution prescribed for preparation of the reference solution. The test is invalid if the monitor solution is not at least as intense as the reference solution.METHOD ATest solution 12 mL of the prescribed aqueous solution of the substance to be examined.Reference solution (standard) A mixture of 10 mL of lead standard solution (1 ppm Pb) R or lead standard solution (2 ppm Pb) R, as prescribed, and2 mL of the prescribed aqueous solution of the substance to be examined.Blank solution A mixture of 10 mL of water R and 2 mL of the prescribed aqueous solution of the substance to be examined.To each solution, add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Examine the solutions after 2 min.System suitability The reference solution shows a slight brown colour compared to the blank solution.Result Any brown colour in the test solution is not more intense than that in the reference solution.If the result is difficult to judge, filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.METHOD BTest solution 12 mL of the prescribed solution of the substance to be examined prepared using an organic solvent containing a minimum percentage of water (for example, dioxan containing 15 per cent of water or acetone containing 15 per cent of water).Reference solution (standard) A mixture of 10 mL of lead standard solution (1 or 2 ppm Pb), as prescribed, and 2 mL of the prescribed solution of the substance to be examined in an organic solvent. Prepare the lead standard solution (1 or 2 ppm Pb) by dilution of lead standard solution (100 ppm Pb) R with the solvent used for the substance to be examined.Blank solution A mixture of 10 mL of the solvent used for the substance to be examined and 2 mL of the prescribed solution of the substance to be examined in an organic solvent.To each solution, add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Examine the solutions after 2 min.System suitability The reference solution shows a slight brown colour compared to the blank solution.Result Any brown colour in the test solution is not more intense than that in the reference solution.If the result is difficult to judge, filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.METHOD CTest solution Place the prescribed quantity (not more than 2 g) of the substance to be examined in a silica crucible with 4 mL of a 250 g/L solution of magnesium sulfate R in dilute sulfuric acid R. Mix using a fine glass rod. Heat cautiously. If the mixture is liquid, evaporate gently to dryness on a water-bath. Progressively heat to ignition and continue heating until an almost white or at most greyish residue is obtained. Carry out the ignition at a temperature not exceeding 800 °C. Allow to cool. Moisten the residue with a few drops of dilute sulfuric acid R. Evaporate, ignite again and allow to cool. The total period of ignition must not exceed 2 h. Take up the residue in 2 quantities, each of 5 mL, of dilute hydrochloric acid R. Add 0.1 mL of phenolphthalein solution R, then concentrated ammonia R until a pink colour is obtained. Cool, add glacial acetic acid R until the solution is decolorised and add 0.5 mL in excess. Filter if necessary and wash the filter. Dilute to 20 mL with water R.Reference solution (standard) Prepare as described for the test solution, using the prescribed volume of lead standard solution (10 ppm Pb) R instead of the substance to be examined. To 10 mL of the solution obtained add 2 mL of the test solution.Monitor solution Prepare as described for the test solution, adding to the substance to be examined the volume of lead standard solution (10 ppm Pb) R prescribed for preparation of the reference solution. To 10 mL of the solution obtained add 2 mL of the test solution.Blank solution A mixture of 10 mL of water R and 2 mL of the test solution.To 12 mL of each solution, add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Examine the solutions after 2 min.System suitability— the reference solution shows a slight brown colour compared to the blank solution,— the monitor solution is at least as intense as the reference solution.Result Any brown colour in the test solution is not more intense than that in the reference solution.If the result is difficult to judge, filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.METHOD DTest solution In a silica crucible, mix thoroughly the prescribed quantity of the substance to be examined with 0.5 g of magnesium oxide R1. Ignite to dull redness until a homogeneous white or greyish-white mass is obtained. If after 30 min of ignition the mixture remains coloured, allow to cool, mix using a fine glass rod and repeat the ignition. If necessary repeat the operation. Heat at 800 °C for about 1 h. Take up the residue in 2 quantities, each of 5 mL, of a mixture of equal volumes of hydrochloric acid R1 and water R. Add 0.1 mL of phenolphthalein solution R and then concentrated ammonia R until a pink colour is obtained. Cool, add glacial acetic acid R until the solution is decolorised and add 0.5 mL in excess. Filter if necessary and wash the filter. Dilute to 20 mL with water R.Reference solution (standard) Prepare as described for the test solution using the prescribed volume of lead standard solution (10 ppm Pb) R instead of the substance to be examined and drying in an oven at 100-105 °C. To 10 mL of the solution obtained add 2 mL of the test solution.Monitor solution Prepare as described for the test solution, adding to the substance to be examined the volume of lead standard solution (10 ppm Pb) R prescribed for preparation of the reference solution and drying in an oven at 100-105 °C. To 10 mL of the solution obtained add 2 mL of the test solution.Blank solution A mixture of 10 mL of water R and 2 mL of the test solution.To 12 mL of each solution, add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Examine the solutions after 2 min.System suitability— the reference solution shows a slight brown colour compared to the blank solution,— the monitor solution is at least as intense as the reference solution.Result Any brown colour in the test solution is not more intense than that in the reference solution.If the result is difficult to judge, filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.METHOD ETest solution Dissolve the prescribed quantity of the substance to be examined in 30 mL of water R or the prescribed volume.Figure 2.4.8.-1. – Apparatus for the test for heavy metalsDimensions in millimetresReference solution (standard) Unless otherwise prescribed, dilute the prescribed volume of lead standard solution (1 ppm Pb) R to the same volume as the test solution.Prepare the filtration apparatus by adapting the barrel of a 50 mL syringe without its piston to a support containing, on the plate, a membrane filter (nominal pore size 3 µm) and above it a prefilter (Figure 2.4.8.-1).Transfer the test solution into the syringe barrel, put the piston in place and then apply an even pressure on it until the whole of the liquid has been filtered. In opening the support and removing the prefilter, check that the membrane filter remains uncontaminated with impurities. If this is not the case replace it with another membrane filter and repeat the operation under the same conditions.To the prefiltrate or to the prescribed volume of the prefiltrate add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately and allow to stand for 10 min and again filter as described above, but inverting the order of the filters, the liquid passing first through the membrane filter before passing through the prefilter (Figure 2.4.8.-1). The filtration must be carried out slowly and uniformly by applying moderate and constant pressure to the piston of the syringe. After complete filtration, open the support, remove the membrane filter, and dry using filter paper.In parallel, treat the reference solution in the same manner as the test solution.Result The colour of the spot obtained with the test solution is not more intense than that obtained with the reference solution.METHOD FTest solution Place the prescribed quantity or volume of the substance to be examined in a clean, dry, 100 mL long-necked combustion flask (a 300 mL flask may be used if the reaction foams excessively). Clamp the flask at an angle of 45°. If the substance to be examined is a solid, add a sufficient volume of a mixture of 8 mL of sulfuric acid R and 10 mL of nitric acid R to moisten the substance thoroughly; if the substance to be examined is a liquid, add a few millilitres of a mixture of 8 mL of sulfuric acid R and 10 mL of nitric acid R. Warm gently until the reaction commences, allow the reaction to subside and add additional portions of the same acid mixture, heating after each addition, until a total of 18 mL of the acid mixture has been added. Increase the amount of heat and boil gently until the solution darkens. Cool, add 2 mL of nitric acid R and heat again until the solution darkens. Continue the heating, followed by the addition of nitric acid R until no further darkening occurs, then heat strongly until dense, white fumes are produced. Cool, cautiously add5 mL of water R, boil gently until dense, white fumes are produced and continue heating to reduce to 2-3 mL. Cool, cautiously add 5 mL of water R and examine the colour of the solution. If the colour is yellow, cautiously add 1 mL of strong hydrogen peroxide solution R and again evaporate until dense, white fumes are produced and reduce to a volume of 2-3 mL. If the solution is still yellow in colour, repeat the addition of 5 mL of water R and 1 mL of strong hydrogen peroxide solution R until the solution is colourless. Cool, dilute cautiously with water R and rinse into a 50 mL colour comparison tube, ensuring that the total volume does not exceed 25 mL. Adjust the solution to pH 3.0-4.0, using short range pH indicator paper as external indicator, with concentrated ammonia R1 (dilute ammonia R1 may be used, if desired, as the specified range is approached), dilute with water R to 40 mL and mix. Add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Dilute to 50 mL with water R and mix.Reference solution (standard) Prepare at the same time and in the same manner as the test solution, using the prescribed volume of lead standard solution (10 ppm Pb) R.Monitor solution Prepare as described for the test solution, adding to the substance to be examined the volume of lead standard solution (10 ppm Pb) R prescribed for the preparation of the reference solution.Blank solution Prepare as described for the test solution, omitting the substance to be examined.Examine the solutions vertically against a white background after 2 min.System suitability— the reference solution shows a brown colour compared to the blank solution,— the monitor solution is at least as intense as the reference solution.Result Any brown colour in the test solution is not more intense than that in the reference solution.If the result is difficult to judge, filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.METHOD GCAUTION: when using high-pressure digestion vessels the safety precautions and operating instructions given by the manufacturer must be followed. The digestion cycles have to be elaborated depending on the type of microwave oven to be used (for example, energy-controlled microwave ovens, temperature-controlled microwave ovens or high-pressure ovens). The cycle must conform to the manufacturer′s instructions. The digestion cycle is suitable if a clear solution is obtained.Test solution Place the prescribed amount of the substance to be examined (not more than 0.5 g) in a suitable, clean beaker. Add successively 2.7 mL of sulfuric acid R, 3.3 mL of nitric acid R and 2.0 mL of strong hydrogen peroxide solution R using a magnetic stirrer. Allow the substance to react with a reagent before adding the next one. Transfer the mixture to a dry high-pressure-resistant digestion vessel (fluoropolymer or quartz glass).Reference solution (standard) Prepare as described for the test solution, using the prescribed volume of lead standard solution (10 ppm Pb) R instead of the substance to be examined.Monitor solution Prepare as prescribed for the test solution, adding to the substance to be examined the volume of lead standard solution (10 ppm Pb) R prescribed for the preparation of the reference solution.Blank solution Prepare as described for the test solution, omitting the substance to be examined.Close the vessels and place in a laboratory microwave oven. Digest using a sequence of 2 separate suitable programmes. Design the programmes in several steps in order to control the reaction, monitoring pressure, temperature or energy depending on the type of microwave oven available. After the first programme allow the digestion vessels to cool before opening. Add to each vessel 2.0 mL of strong hydrogen peroxide solution R and digest using the second programme. After the second programme allow the digestion vessels to cool before opening. If necessary to obtain a clear solution, repeat the addition of strong hydrogen peroxide solution R and the second digestion programme.Cool, dilute cautiously with water R and rinse into a flask, ensuring that the total volume does not exceed 25 mL.Using short-range pH indicator paper as external indicator, adjust the solutions to pH 3.0-4.0 with concentrated ammonia R1 (dilute ammonia R1 may be used as the specified range is approached). To avoid heating of the solutions use an ice-bath and a magnetic stirrer. Dilute to 40 mL with water R and mix. Add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Dilute to 50 mL with water R, mix and allow to stand for 2 min.Filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Carry out the filtration slowly and uniformly, applying moderate and constant pressure to the piston. Compare the spots on the filters obtained with the different solutions.System suitability— the spot obtained with the reference solution shows a brown colour compared to the spot obtained with the blank solution,— the spot obtained with the monitor solution is at least as intense as the spot obtained with the reference solution.Result The brown colour of the spot obtained with the test solution is not more intense than that of the spot obtained with the reference solution. METHOD HTest solution Dissolve the prescribed quantity of the substance to be examined in 20 mL of the solvent or solvent mixture prescribed.Reference solution Dilute the prescribed volume of lead standard solution (10 ppm Pb) R to 20 mL with the solvent or solvent mixture prescribed.Blank solution 20 mL of the solvent or solvent mixture prescribed.To each solution, add 2 mL of buffer solution pH 3.5 R. Mix. (In some cases precipitation occurs, in which case the specific monograph would describe re-dissolution in a defined volume of a given solvent.) Add to 1.2 mL of thioacetamide reagent R. Mix immediately and allow to stand for 2 min. Filter the solutions through a suitable membrane filter (nominal pore size 0.45 µm). Compare the spots on the filters obtained with the different solutions.System suitability The spot obtained with the reference solution shows a brownish-black colour compared to the spot obtained with the blank solution.Result The brownish-black colour of the spot obtained with the test solution is not more intense than that of the spot obtained with the reference solution.Limit Test for Iron(Ph. Eur. method 2.4.9)Dissolve the prescribed quantity of the substance to be examined in water R and dilute to 10 mL with the same solvent or use 10 mL of the prescribed solution. Add 2 mL of a 200 g/L solution of citric acid R and 0.1 mL of thioglycollic acid R. Mix, make alkaline with ammonia R and dilute to 20 mL with water R. Prepare a standard in the same manner, using 10 mL of iron standard solution (1 ppm Fe) R.After 5 min, any pink colour in the test solution is not more intense than that in the standard.Limit Test for Lead in Sugars(Ph. Eur. method 2.4.10)Determine the lead by atomic absorption spectrometry (2.2.23, Method II).Test solution Dissolve 20.0 g of the substance to be examined in a mixture of equal volumes of dilute acetic acid R and water R and dilute to 100.0 mL with the same mixture of solvents. Add 2.0 mL of a clear 10 g/L solution of ammonium pyrrolidinedithiocarbamate R and 10.0 mL of methyl isobutyl ketone R and then shake for 30 s protected from bright light. Allow the layers to separate and use the methyl isobutyl ketone layer.Reference solutions Prepare 3 reference solutions in the same manner as the test solution but adding 0.5 mL, 1.0 mL and 1.5 mL respectively of lead standard solution (10 ppm Pb) R in addition to the 20.0 g of the substance to be examined.Set the zero of the instrument using methyl isobutyl ketone R treated as described for the test solution without the substance to be examined. Measure the absorbance at 283.3 nm using a lead hollow-cathode lamp as source of radiation and an air-acetylene flame.The substance to be examined contains not more than 0.5 ppm of lead, unless otherwise prescribed.Limit Test for Magnesium(Ph. Eur. method 2.4.6)To 10 mL of the prescribed solution add 0.1 g of disodium tetraborate R. Adjust the solution, if necessary, to pH 8.8 to pH 9.2 using dilute hydrochloric acid R or dilute sodium hydroxide solution R. Shake with 2 quantities, each of 5 mL, of a 1 g/L solution of hydroxyquinoline R in chloroform R, for 1 min each time. Allow to stand. Separate and discard the organic layer. To the aqueous solution add 0.4 mL of butylamine R and 0.1 mL of triethanolamine R. Adjust the solution, if necessary, to pH 10.5 to pH 11.5. Add 4 mL of the solution of hydroxyquinoline in chloroform, shake for 1 min, allow to stand and separate. Use the lower layer for comparison. Prepare a standard in the same manner using a mixture of 1 mL of magnesium standard solution (10 ppm Mg) R and 9 mL of water R.Any colour in the solution obtained from the substance to be examined is not more intense than that in the standard.Limit Test for Magnesium and Alkaline-earth Metals(Ph. Eur. method 2.4.7)To 200 mL of water R add 0.1 g of hydroxylamine hydrochloride R, 10 mL of ammonium chloride buffer solution pH 10.0 R, 1 mL of 0.1 M zinc sulfate and about 15 mg of mordant black 11 triturate R. Heat to about 40 °C. Titrate with 0.01 M sodium edetate until the violet colour changes to full blue. To the solution add the prescribed quantity of the substance to be examined dissolved in 100 mL of water R or use the prescribed solution. If the colour of the solution changes to violet, titrate with 0.01 M sodium edetate until the full blue colour is again obtained.The volume of 0.01 M sodium edetate used in the second titration does not exceed the prescribed quantity.Limit test for Heavy Metals in Herbal Drugs and Herbal Drug Preparations(Ph. Eur. method 2.4.27)CAUTION: when using closed high-pressure digestion vessels and microwave laboratory equipment, be familiar with the safety and operating instructions given by the manufacturer.APPARATUSThe apparatus typically consists of the following:— as digestion flasks, polytetrafluoroethylene, perfluoroalkoxy polymer, quartz or glass flasks with a volume of 20-150 mL, fitted with an airtight closure,a valve to adjust the pressure inside the container and a polytetrafluoroethylene tube to allow release of gas;— a system to make flasks airtight, using the same torsional force for each of them;— a programmable microwave oven (e.g. with a magnetron frequency of 2450 MHz, with a selectable output from 0 to 1500 ± 70 W in 1 per cent increments), a polytetrafluoroethylene-coated microwave cavity with a variable speed exhaust fan, a rotating turntable drive system and exhaust tubing to vent fumes;。
欧洲药典7.0附录炽灼残渣 熔点 干燥失重 重金属
熔点：毛细管法测定的熔点是由原来的固体颗粒紧列物质转变为液态时的温度。
专注规定，该装置和方法，用于测定其他因素，如液面凹陷或熔化范围，来描述物质的熔化过程。
装置。
该装置由：-一个合适的玻璃容器含有液体浴（例如，水，液体石蜡或硅油）和安装一个合适的加热装置，-一个合适的手段，搅拌，保证了温度的均匀性的浴室内，-一个合适的温度计毕业不超过0.5摄氏°间隔设有浸泡标记。
一系列的温度不超过100摄氏°，-无碱硬玻璃毛细管内径0.9毫米到1.1毫米与0.10毫米至0.15毫米，壁厚和一端封闭除非另有规定，干燥的细粉状物质在真空和无水硅胶为24小时介绍了足够数量的毛细管管给紧凑型柱4毫米到6毫米的高度。
提高浴的温度约10摄氏°以下的假定的熔点和调整加热速度约1°℃/分钟。
当温度为5℃以下的假定°熔点，正确地介绍了毛细管管插入仪器。
对上述设备，使毛细管管，封闭端附近的中心温度计的灯泡，浸泡标记，是一级液体表面。
记录温度在过去的粒子进入液相校准装置。
该仪器可以校准使用熔点参考物质如世界卫生组织或其他适当的物质。
干燥失重干燥失重质量损失表示质量分数的方法。
将一定量的待测物质在干燥至恒重的称量瓶中检测。
干燥待测物质至恒重或按下列步骤干燥，浮动范围为±2°C。
A, 在干燥器中：常温常压下，以五氧化二磷干燥。
B，真空干燥：室温下，在压强为1.5千帕～2.5千帕，放置五氧化二磷的真空干燥箱内干燥。
C，要求温度范围内真空干燥：在专论规定的温度范围内，压强为1.5千帕～2.5千帕，放置五氧化二磷的真空干燥箱内干燥。
D，在要求温度范围内的干燥箱内干燥：在专论规定的温度范围内干燥E，高真空干燥：在专论规定的温度范围内，压力不超过0.1千帕，放置五氧化二磷的真空干燥箱内干燥。
如有其它要求的条件，根据专论中的具体规定操作。
干燥失重可按下列公式计算：B-C干燥失重（%）= × 100B-AA 称量瓶重量（g）B 干燥前称量瓶与样品的重量（g）C 干燥后称量瓶与样品的重量（g）重金属方法A供试溶液：12ml待测水溶液，2ml pH为3.5的缓冲溶液，混合后加1.2ml 的硫代乙酰胺试液，立即混合。
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第二部分、附录附录1 溶液的澄清度 (2)附录2 溶液颜色检查 (2)附录3 旋光度 (6)附录4 铵盐检查法 (8)附录5 氯化物检查法 (9)附录6 硫酸盐灰分 (10)附录7 铁 (11)附录8 重金属 (12)附录9 干燥失重 (15)附录10 硫酸盐检查法 (16)附录11 红外吸收分光光度法 (17)附录12 pH测定 (20)附录13 滴定 (22)附录14 氯化物鉴别反应 (23)附录15 指示剂颜色与溶液pH 的关系 (24)附录1 溶液的澄清度在内径15～25mm，平底，无色、透明、中性玻璃管中，加入等量的供试溶液与浊度标准液，使液位的深度都为40mm，按如下所述方法进行比较。
浊度标准液制备5分钟后，以色散自然光照射浊度标准溶液和供试溶液，在黑色背景下从垂直方向观察、比较澄清度或浑浊程度。
色散自然光必须较容易区分浊度标准溶液Ⅰ与水，浊度标准溶液Ⅱ与浊度标准溶液Ⅰ。
如果供试溶液的澄清、透明程度与水相同，或者与所用溶剂相同，或者其澄清度不超过Ⅰ号浊度标准溶液，那么可判定该溶液为澄清。
试剂：硫酸肼溶液：取1.0g硫酸肼溶于水，加水稀释至100.0ml，静臵4～6小时。
乌洛托品（六亚甲基四胺）溶液：在100ml容量平中，以25.0ml水溶解2.5g乌洛托品。
浊度标准贮备液：在存放乌洛托品溶液的100ml容量瓶中，加25.0ml的硫酸肼溶液。
混合，静臵24小时，贮存在无表面要求的玻璃容器中，可在2个月内使用。
该浊度液不得黏附玻璃，用前必须充分摇匀。
浊度标准原液：取浊度标准贮备液15ml，加水稀释、定容至1000ml。
该液临用前制备，至多保存24小时。
浊度标准液：由浊度标准原液与水按表1-1配制,即得。
本液应临用前配制。
附录2 溶液颜色检查按本药典规定，用下面两种方法之一可以检出溶液在棕色-黄色-红色范围内的颜色。
如果溶液A的外观与水或所用溶剂相同，或者颜色浅于标准比色液B9，则可判定溶液A为无色。
方法I用外径为12mm的无色、透明中性玻璃管取2ml的供试溶液，与相同玻璃管中的2ml的水，或2ml本文所规定的标准比色液（见标准比色液表）进行比较。
在散射自然光，白色的背景下，水平观察比较颜色。
方法Ⅱ用同样平底、内径为15～25mm的无色透明中性玻璃管，液位的深度为40mm，将供试溶液与水或溶剂或本文中规定的标准比色液（见标准比色液表）对比。
在散射自然光，白色的背景下，垂直地观察比较颜色。
贮备液黄色液称取46克氯化铁，加大约900ml盐酸溶液（25ml浓盐酸和975ml 水混和）溶解，继续添加，并定容1000.0ml。
滴定并以上述盐酸溶液调整，使黄色液每毫升含45.0mg FeCl3﹒6H2O。
避光保存。
滴定在一个配有磨口塞的250ml锥形瓶内，加入10.0ml黄色液，15ml 水，5ml浓盐酸和4g碘化钾，塞上瓶塞，在暗处放臵15分钟，再加100ml 水。
用0.1M的硫代硫酸钠标准溶液滴定游离的碘，在滴定接近终点时加0.5ml淀粉试液作指示剂。
1ml 0.1M的硫代硫酸钠标准溶液相当于27.03mg FeCl3﹒6H2O。
红色液称取60克氯化钴，加大约900ml盐酸溶液（25ml浓盐酸和975ml 水混和）溶解，继续添加，并定容1000.0ml。
滴定并以上述盐酸溶液调整，使红色液每毫升含59.5mg CoCl2﹒6H2O。
滴定在一个配有磨口塞的250ml锥形瓶内，加入5.0ml红色液，5ml稀过氧化氢溶液和10ml 300g/l的氢氧化钠溶液，缓慢煮沸10分钟，冷却后，加60ml 稀硫酸和2g碘化钾，塞上瓶塞，缓慢摇动锥形瓶，使沉淀溶解完全。
用0.1M 的硫代硫酸钠标准溶液滴定游离的碘，在滴定接近终点时加入0.5ml淀粉试液作为指示剂。
溶液变成粉红色时到达滴定终点。
1ml0.1M的硫代硫酸钠标准溶液相当于23.79mg CoCl2﹒6H2O。
蓝色液称取63克硫酸铜加大约900ml盐酸溶液（25ml浓盐酸和975ml水混和）溶解，继续添加，并定容1000.0ml。
滴定并以上述盐酸溶液调整，使蓝色液每毫升含62.4mg CuSO4﹒5H2O。
滴定在一个配有磨口塞的250ml锥形瓶内，加入10.0ml蓝色液，50ml水，12ml稀醋酸和3g碘化钾。
用0.1M的硫代硫酸钠标准溶液滴定游离碘，在滴定接近终点时加入0.5ml淀粉试液作为指示剂。
当溶液变为轻微的淡褐色时到达滴定终点。
1ml0.1M的硫代硫酸钠标准溶液相当于24.97mg CuSO4﹒5H2O。
颜色标准溶液用3种贮备液制备5种颜色标准液。
如表2-1。
方法I和方法Ⅱ的标准比色液用5种颜色标准溶液，制备以下各种颜色的标准比色液。
储存对于方法I，标准比色液在外径为12mm的无色透明中性封口的玻璃管中储存，避光。
对于方法Ⅱ，使用前直接从颜色标准液制备标准比色液。
仪器和试剂：附录3 旋光度旋光是手性物质的特性，即能使偏振光的平面旋转。
右旋物质的旋光度为正的（+），即右旋物质可以使偏振光平面顺时针方向旋转；左旋物质的旋光度为负的（-）。
精确的旋光度是指,在温度t下，波长为λ的光透过长1m或含1kg/m3旋光活性物质的液体，所发生的旋转，用弧度(rad)表示。
实际操作中，旋光度常用mrad ﹒m2﹒kg-1表示。
本药典采用以下常规定义纯液体旋光度：旋光度以角度(°)表示，即20℃下，1dm长测定管的纯液体使钠光谱D线（λ＝589.3nm）的偏振光平面所旋转的角度；对于溶液，按专论规定方法制备。
液体旋光度：测定即20℃下，1dm长的测定管的含待测液体的溶液使钠光谱D线（λ＝589.3nm）的偏振光平面所旋转的角度(°)，即溶液旋光度。
溶液中液体旋光度，由溶液旋光度除以溶液中被检测液体的密度（g/cm3）计算得出。
固体物质的旋光度：测定20℃下，1dm长测定管的含被测物质1g/ml的溶液使钠光谱D线（λ＝589.3nm）的偏振光平面所旋转的角度，即溶液旋光度。
溶液中固体物质的旋光度由溶液的旋光度计算得出。
溶液中某物质的旋光度与溶剂和浓度有关。
按本药典采用的惯例，旋光度不标注单位；它的实际单位为(°)﹒ml﹒dm-1﹒g-1。
本药典的旋光度同国际标准单位旋光度的换算关系如下：如果专论有特别要求，按要求选择温度（可能不是20℃）和波长。
旋光计的读数必须精确到0.01°。
测量范围通常由鉴定用石英片检查；测量范围内线性由蔗糖溶液检查。
方法20±0.5℃下，旋光计调零，用钠光谱的D线（λ＝589.3nm）测定，或者按专论要求的温度测定旋光度。
测定液体的旋光度，测定前放入封闭的空测定管，调零；测定固体的旋光度，测定前放入盛有所用溶剂测定管，调零。
按下式计算旋光度：纯液体旋光度：溶液中物质的旋光度：c为浓度，单位g/l。
按下式计算以g/l为单位的溶解物质的浓度c，或以m/m百分比为单位的浓度c′：= 20 ± 0.5°C下，旋光度读数，单位度（°）l = 测定管长度，单位dm。
ρ20 = 20 °C 下溶液密度，单位g/cm3,本药典在2.2.5节中以相对密度代替密度。
c = 溶解物质的浓度，单位g/l。
c′ = 溶解物质的浓度，单位g/l。
除非另有规定，通常用方法A。
方法A供试溶液：在比色管中用14ml水溶解规定质量的供试品，必要时加入稀释的氢氧化钠溶液使溶解，用水稀释至15ml。
再加0.3ml碱性碘化汞钾试液。
标准溶液：取10ml的标准铵溶液(1ppmNH)，加5ml水和0.3ml碱性碘化汞4钾试液。
两溶液摇匀后分别用塞子塞住比色管。
5分钟后，供试溶液中的黄色不得比标准溶液中的颜色更深。
方法B在25ml有盖子2的广口瓶中，加入规定数量的供试品细粉，使其溶解或悬浮在1ml的水中，加0.30g重氧化镁。
取一片5mm的正方形银锰纸，滴几滴水使其湿润，铺在瓶口，然后立即盖上聚乙烯瓶盖。
漩涡混和，防止液体溅出，在40℃下放臵30分钟。
如银锰纸显示灰色，其颜色不得比，规定量的标准铵溶液（1ppmNH4），加1ml的水，0.3克氧化镁制成的标准溶液的银锰纸的颜色更深。
供试溶液：15ml待测溶液，加1ml稀硝酸于测试管中，混合，然后将混合溶液倒入装有1ml硝酸银溶液的比色管中。
标准溶液：10ml的氯化物标准液（5ppm Cl），加5ml水，加1ml稀硝酸，混合，然后将混合溶液倒入装有1ml硝酸银溶液的比色管中。
黑色背景下对比两份溶液的颜色。
避光放臵5分钟后，供试溶液中的乳白色不得比标准溶液更深。
附录6 硫酸盐灰分将坩埚（由铂、瓷或石英制成）在600±50℃灼烧30分钟，取出放入已放臵硅胶的干燥器内，冷却后称重。
将规定量的供试品臵于上述坩埚内，称重。
加少量硫酸（通常1ml）湿润供试品，按要求温度缓慢加热，直至供试品完全炭化。
冷却后，加少量硫酸润湿残渣，继续加热到没有白烟冒出。
再在600±50℃灼烧至完全灰化。
操作过程中应避免燃着。
取出坩埚臵于已放臵硅胶的干燥器内冷却，冷却后称重，计算残渣的重量。
如果残渣超过规定，除有其他规定，重复以上操作，直至恒重。
附录7 铁供试溶液:将规定数量的供试品溶于水中，并用水稀释至10ml,或者直接用10ml规定溶液。
加2ml 200g/l的柠檬酸溶液和0.1ml的硫醇基乙酸（硫乙醇酸），混合，加氨水使偏碱性，再用水稀释至20ml。
供试溶液：10ml的标准铁溶液（1ppm Fe）按供试溶液的方法制备成20ml 标准溶液，5分钟后，供试溶液中的粉红色不得比标准溶液深。
附录8 重金属方法A供试溶液：12ml待测水溶液，2ml pH为3.5的缓冲溶液，混合后加1.2ml的硫代乙酰胺试液，立即混合。
对照溶液：10ml的标准铅溶液（1ppm or 2ppm Pb）， 2ml pH为3.5的缓冲溶液，2ml的待测液，混合后加1.2ml的硫代乙酰胺试液，立即混合。
空白溶液：10ml的水，2ml pH为3.5的缓冲溶液，2ml的测试溶液。
混合后加1.2ml的硫代乙酰胺试液，立即混合，同空白溶液比较，对照溶液显浅棕色。
2分钟后，供试的溶液颜色不得比对照溶液深。
方法B用含最少量水的溶剂（例如含15％水的二氧杂环乙烷或含15％水的丙酮）溶解规定量的供试品，制成待测液供试溶液：12ml待测液， 2ml pH为3.5的缓冲溶液，混合后加1.2ml的硫代乙酰胺试液，立即混合。
对照溶液：10ml的标准铅溶液（1ppm or 2ppm Pb）， 2ml pH为3.5的缓冲溶液， 2ml的待测液，混合后加1.2ml的硫代乙酰胺试液，立即混合。
空白溶液：10ml的水，2ml pH为3.5的缓冲溶液，2ml的测试溶液。
混合后加1.2ml的硫代乙酰胺试液，立即混合，同空白溶液比较，对照溶液显浅棕色。