chp03 Pro-treatment of sample.ppt

Chapter 3 Sample preparation andValidation of analytical method Section 1 Work-up procedures prior to analysis ——Sample preparation 1.1 General Considerations Halogen-containing drugs ——organic halides, halogenides Organo-metal drugs (organometallic drugs) ——organic metals ——metal-containing compounds (organic metallic salts) Organic halides 泛影酸 碘番酸 三氯叔丁醇 磺溴酞钠 Organic metals 酒石酸锑钾 富马酸亚铁 Metal-containing compounds 卡巴胂 1.2 Determination non-organic degradation (1) direct determination such as: Ferrous fumarate — may dissolve in hot diluted mineral acid and yield the ferrous ion, can be titrated using ceric sulfate VS. **cerium(Ⅲ), ceric(Ⅳ,高价), cerous(Ⅱ,低价). (2) determination after hydrolysis (reflux) application: the halogen was not firmly connected to drug —— to halogen no double bonded carbon atom was connected (aliphatic halide). ① alkaline hydrolysis Dissolve organic halide in a suitable Solution, such as alcohol, add sodium hydroxide solution or silver nitrate VS, reflux to make organic halide change into inorganic halide (NaX or AgX), then (add AgNO3VS) titrate using the ammonium thiocyanate (NH4SCN) VS. for example: determination of Chlorobutanol ② acid hydrolysis,such as magnecium stearate (3) Determination after oxido-reduction application: iodine-containing compound that iodine was firmly connected to double-bonded carbon atom — benzene ring ① alkaline reduction dissolve organic halide in a sodium hydroxide solution (