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本文介绍一种测定可待因的分光光度法,此法系基于可待因与溴甲酚绿(1:1)作用生成黄色复合物,其在pH3.8的氯仿抽提液于418nm波长处有最大吸收。复合物可稳定10天,并在3～12μg/ml浓度范围内符合比尔定律。制剂中的赋形剂、色素、调味剂及其它药物如片剂中的乙酰水杨酸(20mg)、咖啡因(0.1g)、苯巴比妥(20mg);糖浆中的盐酸去氧肾上腺素(2mg)、氯化铵(30mg)、薄荷脑(30mg)、苯甲酸钠(15mg)、甘油(10mg)、乙醇(5mg)、糖精钠(30mg)、扑热息痛(20mg)、愈创木酚磺酸钾(50mg)、苋菜红(20mg)在不超过一定限量(即以上括号中所示的量)的情况下对本法无干扰。如含有盐酸麻黄碱、安替比林、抗组胺药及含有叔胺基团或季铵盐的药物可按下述薄层层析法分离后测定。表中列出可待因的回收率(从略)。试剂:所有溶液均用分析纯试剂配制。pH3.8缓冲溶液(英国药典标准);可待因缓冲溶液(取69.84mg溶于N/10氢氧化钠液2ml,用上述缓冲溶液稀释至1000ml)。操作方法:吸取上述可待因液3ml,置50ml分液漏斗中,加溴甲酚绿液20ml,产生的黄色复合物分次用氯仿5ml、3ml、2ml剧烈振摇提取,提取液收集于10ml量瓶中,加氯仿至刻度,于418nm波长处测定吸收度,以氯仿作空白。样品检验:取含有可待因100μg及通常与可待因配伍的各种药物的混合溶液,按上述操作方法检验即可。如有干扰,可先用硅胶进行薄层层析。取一定体积含有可待因约4mg的药物制剂,以4N氢氧化钠液碱化,用氯仿抽提五次,每次10ml,抽提物进行层析(乙酸乙酯-甲醇-氨水=75:15:10),分离所得可待因溶于N/10盐酸液,以N/10氢氧化钠液中和,置250ml量瓶中,用缓冲溶液稀释至刻度,吸取一定量按上述操作方法进行检验。本法优点是简单灵敏,可用于一些药物制剂中的可待因测定。
This article describes a spectrophotometric method for the determination of codeine based on the action of codeine and bromocresol green (1: 1) to produce a yellow complex with a chloroform extract at pH 3.8 at 418 nm Have the greatest absorption. The complex is stable for 10 days and complies with Beer’s law at concentrations ranging from 3 to 12 μg / ml. (20mg), caffeine (0.1g), phenobarbital (20mg) in tablets, phenylephrine hydrochloride in syrup (2 mg), ammonium chloride (30 mg), menthol (30 mg), sodium benzoate 15 mg, glycerol 10 mg, ethanol 5 mg, sodium saccharin 30 mg, Potassium (50mg), Amaranth (20mg) This method does not interfere with this limit if it does not exceed a certain limit (that is, the amount shown in brackets above). For example, drugs containing ephedrine hydrochloride, antipyrine, antihistamines and tertiary amine groups or quaternary ammonium salts may be separated and determined by the following thin-layer chromatography. The table lists the recovery of codeine (omitted). Reagents: All solutions are prepared using analytical reagents. pH3.8 buffer solution (British Pharmacopoeia standard); codeine buffer solution (take 69.84mg dissolved in 2ml of N / 10 sodium hydroxide solution and dilute to 1000ml with the above buffer solution). Method of operation: draw the codeine liquid 3ml set 50ml separatory funnel, bromocresol green solution 20ml, the resulting yellow complex fractionated with chloroform 5ml, 3ml, 2ml vigorously shaking extract, the extract collected in 10ml Volumetric flask, plus chloroform to the mark, absorbance was measured at a wavelength of 418nm, with chloroform as a blank. Sample test: Take codeine containing 100μg and usually with codeine compatibility of various drugs mixed solution, according to the above method of operation can be tested. If there is interference, first silica gel TLC. Take a certain volume of drug formulation containing codeine about 4mg, basified with 4N sodium hydroxide solution, extracted five times with chloroform, 10ml each time, the extract was chromatographed (ethyl acetate - methanol - ammonia = 75: 15:10), the resulting codeine was dissolved in N / 10 hydrochloric acid solution, with N / 10 sodium hydroxide solution and set 250ml volumetric flask, dilute to the mark with a buffer solution, to absorb a certain amount according to the above method of operation test. The advantages of this method is simple and sensitive, can be used for the determination of codeine in some pharmaceutical preparations.