药科大学教案-(药物分析试验首页1)

中国药科大学教案(药物分析试验首页1)实验一葡萄糖的性状、鉴别和检查教学目的1、了解药品鉴别、检查的目的和意义；2、掌握药品性状测定方法和性状的正确描述；3、掌握药品的常用鉴别的方法和原理；4、掌握药品中一般杂质检查的方法原理和限量计算方法。

本章讲授提纲及学时分配【性状】本品为无色结晶或白色结晶性或颗粒性粉末；无臭，味甜。

溶解性―――――――结构式分析（60min）比旋度测定依中国药典2000年版二部附录ⅥE测定，比旋度为＋52.5°至＋53.0°。

―――――旋光仪使用（120min）【鉴别】(1)碱性酒石酸铜试液，生成氧化亚铜的红色沉淀。

――――――化学反应式（60min）【检查】――――――各检查的注意事项（120min）酸度加水20ml溶解，加酚酞指示液与氢氧化钠滴定液，应显粉红色。

氯化物依中国药典2000年版二部附录ⅧA检查，与标准氯化钠溶液6.0ml制成的对照液比较，不得更浓(0.01％)。

重金属依中国药典2000年版二部附录ⅧH第一法检查，含重金属不得过百万分之五。

砷盐依法中国药典2000年版二部附录ⅧJ第一法检查，应符合规定(0.0001％)。

教学参考书中国药典2000年版二部本章内容的重点旋光仪的使用比色管的使用及清洗一般杂质限量的计算本章内容的难点古蔡氏试砷法中所加各试剂的作用与操作注意点复习思考题1、鉴别检查在药品质量控制中的意义及一般杂质检查的主要项目是什么?2、比色比浊操作应遵循的原则是什么?3、试计算葡萄糖重金属检查中标准铅溶液的取用量。

4、古蔡氏试砷法中所加各试剂的作用与操作注意点是什么?5、根据样品取用量、杂质限量及标准砷溶液的浓度，计算标准砷溶液的取用量。

教具及教学设备要求100ml容量瓶，10ml离心管，旋光仪，纳氏比色管，试砷瓶。

Experiment 1 The Description，Identification and Tests ofGlucoseI. Purpose1.To understand the aims and purposes of the drug quality control.2.To learn about the methods for the determination and the special words for the descriptionof the characteristics of drugs.3.To experiment on the identification of glucose.4.To study and experiment on the methods of drug tests2. Contents and teach time assignmentDescription Colourless crystals or a white crystalline or granular powder；odourless；taste, sweet. Dissolubility--------------------------------(60min)Specific optical rotation Polarimeter --------------------------------(120min)Identification announcements--------------------------------(60min)(1) Dissolve about 0.2 g in 5 ml of water，add dropwise hot alkaline cupric tartrate TS；a redprecipitate of cuprous oxide is produced.examination ------------------------------(120min)Acidity Dissolve 2.0 g in 20 ml of water, add 3 drops of phenolphthalein IS and 0.20 ml of sodium hydroxide (0.02 mol/L) VS; a pink colour is produced.Chloride Carry out the limit test for chlorides (Appendix VIII A)，using 0.60 g. Any opalescence produced is not more pronounced than that of a reference using 6.0 ml of sodium chloride standard solution (0.01%).Heavy metals Dissolve 4.0 g in 23 ml of water，add 2 ml of sodium acetate BS (pH 3.5)，carry out the limit test for heavy metals (Appendix VIII H，method 1): not more than 0.0005%. Arsenic(Appendix VIII J，method 1) (0.0001%).Referencesthe Volumn 2 of Chinese PharmacopoeiaFocal pointThe use of PolarimeterHow to use and clear the color comparison tubeHow to figure out the limit of arsenic or heavy matalsDiscussion1.What are the purposes of drug identification and test? What are the usual items of drugtests?.2.What are the standard operation procedures for the clarity test?3.How much of the lead standard solution should be taken for the limit test for heavymetals in this experiment?4.What precautions should be taken for the limit test for arsenic(Appendix VIII J，method1)? And what is the function for each of the test solutions added?5.Figure out the amount of the arsenic standard solution that should be taken for the limittest for arsenic(Appendix VIII J，method 1) (0.0001%) in this experiment with the specified quantity of 2.0 g of sample.teaching device100ml volumetric flask; 10ml centrifuge tube; polarimeter; color comparison tube; arsenictest bottle实验二阿司匹林及阿司匹林肠溶片的质量分析教学目的1.掌握质量检验的项目与方法；2.掌握阿司匹林及阿司匹林肠溶片分析的操作条件及要点。

本章讲授提纲及学时分配【性状】本品为白色结晶或结晶性粉末；无臭或微带醋酸臭，味微酸；遇湿气即缓缓水解。

溶解性―――――――结构式分析（30min）【鉴别】(1)取本品约0.1g，加水10ml，煮沸，放冷，加三氯化铁试液1滴，即显紫堇色。

(2)取本品约0.5g，加碳酸钠试液10ml，煮沸2分钟后，放冷，加过量的稀硫酸，即析出白色沉淀，并发生醋酸的臭气。

――――――化学反应式（1hour）【检查】――――――各检查的注意事项（1hour）溶液的澄清度取本品0.50g，加温热至约45℃的碳酸钠试液10ml溶解后，溶液应澄清。

游离水杨酸新制的稀硫酸铁铵溶液、硫酸铁铵指示液显色，与对照液(精密称取水杨酸配制)比较，不得更深(0.1％)。

【含量测定】―――――――（5.5hour）原料中性乙醇溶解后，加酚酞指示液3 滴，用氢氧化钠滴定液直接滴定。

片剂两步滴定法。

本课程学科的新进展与理论课相结合，再复习阿司匹林的各种含量测定法，相关文献介绍。

教学参考书中国药典2000年版二部本章内容的重点原料与片剂为何要用不同的测定含量方法本章内容的难点中性乙醇的制备，两步滴定法的操作注意点本章内容及讲授的改进意见复习思考题1.阿司匹林原料药物与及阿司匹林肠溶片在质量检验方面有哪些不同之处？为何不同？2.阿司匹林肠溶片释放度检查中为什么要更换溶剂？教具及教学设备要求50ml烧杯，10ml离心管，电炉，水浴锅，滴管，滴定管。

Experiment 2 The Analysis of Aspirin and AspirinEnteric-coated TabletsI. Purpose1.To learn about the procedures and the items for drug analysis.2.To experiment on the analysis of Aspirin and its Enteric-coated Tablets.2. Contents and teach time assignmentDescription Dissolubility--------------------------------(30min)Identification announcements--------------------------------(1hour)(1) To about 0.1 g add 10 ml of water，boil and cool. Add 1 drop of ferric chloride TS；a violet colour is produced.(2) To about 0.5 g add 10 ml of sodium carbonate TS，boil for 2 minutes and cool. Add dilute sulfuric acid in excess；a white precipitate is produced and an odour of acetic acid is perceptible. Examination ------------------------------------------(1hour)Clarity of solutionSalicylic acidAssay -------------------------------------(5.5hour)Material direct titration using sodium hydroxideTablet two-step titration.Referencesthe Volumn 2 of Chinese PharmacopoeiaFocal pointThe preparation of neutro- alcoholHow to operate tow-step titrationDiscussion1.What is the difference between the assay of aspirin and its enteric-coated tablets?2.Give an explanation of the purpose of the solvent changing during the drug release testof aspirin enteric-coated tablets.teaching device50ml beaker;10ml centrifuge tube . electric furnace , thermostat-controlled waterbath, volume buret实验三复方磺胺甲噁唑片的质量分析教学目的1.熟悉复方制剂双波长计算分光光度方法含量测定原理；2.掌握复方磺胺甲噁唑片实验的操作条件及要点。