山道年的比色测定方法 Ⅰ.三氯化铁法

山道年(Santonin)的含量测定,文献所载有容量法、旋光法、重量法等,但一般采用的仍偏重于重量法。Fromme的结晶法至今仍被广泛采作依据。但在分析结果上有的方法需要加校正数,有的用样品量很大,费时亦长。近年来关于山道年的比色方法作了不少工作,日人山口一孝与山岸正治曾进行了2,4二硝基苯肼比色法,前者利用山道年与2,4二硝基苯肼作成苯腙沉淀然后溶解比色,后者利用山道年与2,4二硝基苯肼作成苯腙,不需沉淀及滤取,放置一夜后,通过填满氧化铝之吸附柱,     

合剂中山道年的极谱分析法

山道年及其制剂的分析法,有抽出后称重法,水解后滴定法,抽出后用2、4二硝基苯肼沉淀法,比色法等,此等方法,或操作麻煩,或所得結果很难准确,尤其是宝塔糖等赋料甚多的合剂,更無較好的方法。根据Santavy氏的报告,在含水酒精溶液中,可用極譜法测定山道年;在山道年、酚酞、糖、乳糖及可可的混合物中,用酒精抽取后,以硫酸鋰为支持电解質,可直接测定     

两种旋光性物质浓度和旋光度的关系式——应用于盐酸麻黄硷总量和左、右旋体含量的测定

1-麻黄硷和d-伪麻黄硷是麻黄中的主要成分,提取时主要是此两种生物硷的混旋体。测定该混旋体的方法有数种。例如用氯仿提取d-盐酸伪麻黄硷(或称盐酸异麻黄硷)的重量分析法;М.И.Горяеь等利用左、右旋麻黄硷的草酸盐溶解度不同的分离测定法。近来用分光旋光法根据不同波长和不同溶质浓度时,左、右旋麻黄硷的旋光度有所改变,所进行的1-和d-伪麻黄硷的测定,适用于低含量样品的测定。旋光法测定对映体混合物的方法基本有     

自蛔蒿提取山道年方法的研究

本吱报导了两个自(虫冂日)蒿(Artemisia incana Keller)提取山道年的方法。一法系将浓缩的石灰水抽出液酸化后用苯萃取,苯溶液通过氧化铝吸附柱精制,收率为83—85%。一法系将浓缩的石灰水抽出液用硫酸酸化,析出的粗山道年用碱水洗后,以15%乙醇重结晶精制,收率为73—76%,两法所得山道年的质量,皆符合于我国药典(1953年版)的规格。     

旋光法测定盐酸阿糖胞苷滴眼液的含量

盐酸阿糖胞苷滴眼液的含量测定常采用提取后分光光度法、双波长分光光度法等,该法虽结果比较准确,但操作比较费时,又受仪器限制,不适应基层单位快速测定的需要。根据盐酸阿糖胞苷具有旋光性的特点(比旋度 127°～ 133°),本文试用旋光法测定盐酸阿糖胞苷滴眼液的含量,结果表明本法快速简便,回收率高,有一定实用价值。     

山道年及其异构体的高效液相色谱分析

α-山道年是从菊科植物蛔蒿(Artemisia cina Berg.)未开放的花蕾中提取的一种内酯,为有效的驱蛔药物,而东北蛔蒿(Artemisia incana Keller.)中则含有β-山道年。β-山道年的驱蛔效力较弱。药典中山道年的含量测定方法只能测定其总量,而不能区分异构体。 里田 勳等曾用气相色谱法;黑田辰一郎用红外吸收光谱法;罗淑荣等用薄层     

茴蒿的快速极谱分析

茴篙是驱蛔虫的药用植物,其中主要有效成分是山道年.因此茴蒿中山道年的含量测定在茴蒿的选种、栽培、采集时间、以及提取和制备山道年的过程中都是很重要的.但是一般的测定方法都比较费时费事.根据山道年在滴汞电极上的可还原性,曾有不少作者拟出山道年在制剂中的极谱测定方法,但尚没有一个比较理想的茴蒿分析方法.我们在对山道年和山道年酸进行了一系列的观察以后,参考自茴蒿中提取山道年的方     

硅钨酸沉淀法测定盐酸硫胺含量的改进

盐酸硫胺含量的测定方法,文献报道不下数十种,归纳起来可以分为三类:(一)仪器法,(二)容量法,(三)重量法。仪器法又分为分光光度法与萤光光度法。三类方法各有优缺点和适用范围。仪器法快速、选择性高,但需专用仪器和校正物质,误差也较大,常用于复方维生素B制剂的测定(分光法需先经过离子交换树脂的处理,将干扰物质分离)。容量法如非水碱量法、银量法等,有快速、简单、不需要贵重仪器等优点,缺点是选择性不高,仅适用于纯品的快速测定。重量法(硅钨     

复方乳酸钠注射液中葡萄(米广)含量测定的实验

碘量法是医院药房在无旋光仪的条件下,测定液中菊萄精的含量时,和旋光法基本一致。但我们在实际工作中发现用于测定复方乳酸钠注射液(用115.5’灭菌30分钟)中葡萄糖含量时,和旋光法比较有效大差别,现将实验结果列表如下;附表工蔺箱含盆洲定的结果!含量(标示量肠),注射液名称{灭菌前灭菌后旋光法碘量法旋光法碘量法‘。雳夏纂     

络合滴定法在有机藥物分析中的应用 Ⅲ.阿的平及其制剂的含量测定

阿的平(Atebrine)为治疗虐疾的重要药物,虽未收载于我国药典中,但已为较多国家的药典所收载,其含量测定方法在文献中记载的有:重铬酸盐沉淀容量法、矽钨酸滴定法、分光光度法、离子交换法、氯化碘容量法、硷量法,以及提取游离硷重量法等,其中提取游离硷重量法及重鉻酸盐沉淀容量法虽已为若干国家药典采用为法定方法,但前者需干燥至恆重,消耗时间较久;而后者由于阿的平一重铬酸盐的溶解度较大,     

碱性锌还原法测定3-乙酰氨基-2,4,6三碘苯甲酸(乌乐康)的碘含量

肾造影剂3-乙酰氨基-2,4,6三碘苯甲酸(鸟乐康),其碘含量测定的方法,美典XV版⑴及N.N.R.⑵都采用鹼性溶液中以高锰酸钾氧化法(该药品种较新尚未见诸其他药典),这个方法的缺点是分析週期太长(需在水浴上迥流18小时),有时尚有偏低的现象,由于存在上述缺点,故不能适应车间生产上的需要。     

抗疟药物非水溶液滴定法之研究

本文报告了一个簡單快速而准确的非水溶液滴定法测定抗瘧药物片剂,用以测定十一种抗瘧药物片剂,所得的結果与药典方法符合。     

麻黄生药中麻黄硷的非水溶液滴定法

麻黄生药中麻黄硷的含量测定,各国药典上所采用的方法都很复杂,费时间。近年来用非水溶液滴定法来测定许多生物硷,可以大大简化测定的手续,节省了时间。Chatten和Pernarowski二氏曾用过氯酸的冰醋酸溶液直接滴定滴鼻剂中的麻黄硷,或先用氯仿抽出,再用过氯酸的冰醋酸溶液滴定。此法简便,迅速,依理可作为测定麻黄生药中麻黄硷的方法,但是生药中成分复杂,能溶于氯仿中的物质很多,可以干扰满定终点,因此需要     

使君子酸钾对人体蛔虫驱除效力的初步报告

使君子对人体具有驱除蛔虫的效力,已属定论.作者陈、李曾从使君子内提炼得一结晶性物质,命名为使君子酸钾;经药理初步试验,证明对蚯蚓显示毒效,具有驱虫效力。为了进一步证实此物质对人体蛔虫是否确具驱除效力起见,作者在1949年进行了临床试用.本试验在一女童教养所进行.学生204人,均在同一环境条件生活及成长。粪便经虫卵常规检查,发现均有蛔虫寄生.为了便于比较驱虫效力,一部分患者采用了山道年进行治疗.为了说明使君子酸钾的驱虫效力,以及它是否为使君子中的有效成分,采     

Synthesis of <Emphasis Type="Italic">C</Emphasis><Subscript>6</Subscript>-epimer derivatives of diacetoxy acetal derivative of santonin and their inducing effects on HL-60 leukemia cell differentiation

Induction of differentiation is a new and promising approach to leukemia therapy, well illustrated by the treatment of acute promyelocytic leukemia with 1,25-dihydroxyvitamin D₃ [1,25-(OH)₂D₃] or all-trans retinoic acid (ATRA). Using combination of either 1,25-(OH)₂D₃ or ATRA and chemotherapy, adverse effects 1,25-(OH)₂D₃ or ATRA such as hypercalcemic effects have decreased, and long-term survival has improved. In a previous study, we demonstrated that santonin could be chemically modified into a diacetoxy acetal derivative of santonin with strong differentiation-inducing activity. In this study, we further synthesized C₆-epimer derivatives of diacetoxy acetal derivative of santonin and tested their effects on HL-60 cell differentiation. Some of the C₆-epimer derivatives themselves induced increases in cell differentiation. Especially, (11S)-3,3-(ethylenedioxy) eudesmano-13-ol-6β-acetate (7) was demonstrated to induce differentiation with larger than 80% of the cells attaining a differentiated phenotype. Importantly, 7 strongly enhanced differentiation of HL-60 cells in a dose-dependent manner when combined with either low doses of 1,25-(OH)₂D₃ or ATRA. The ability to enhance the differentiation potential of 1,25-(OH)₂D₃ or ATRA by 7 may improve outcomes in the therapy of acute promyelocytic leukemia.     

A method for the estimation of the catecholamines and their metabolites in brain tissue

1. A method is described whereby the catecholamines, their precursors and metabolites may be estimated in the same brain sample. The method, outlined below, was rigorously tested in pure solution before being applied to the estimation of the catechol and methoxyamines in extracts of rat brain. (i) The brain tissue was homogenized in perchloric acid and the perchloric acid removed as its insoluble potassium salt. (ii) The acid metabolites of the amines were extracted from the acidified extract into ethyl acetate. (iii) After extraction with ethyl acetate, the aqueous extract was treated with acetic anhydride and sodium hydrogen carbonate and the acetylated derivatives of the amines extracted into dichloromethane. (iv) The aqueous solution remaining after extraction with dichloromethane contains the acetylated amino-acids. Acetyl-dopa could be extracted into dichloromethane only after acidification of this aqueous solution. The acetyl-dopa in this dichloromethane extract could be estimated fluorimetrically. (v) The dichloromethane extract containing the acetylated amines was chromatographed on paper in the organic phase of a mixture of toluene:ethyl acetate:methanol:water, 10:1:5:5. (vi) The acetylated amines were eluted and estimated fluorimetrically. A new method was developed for the estimation of 3-methoxytyramine and its acetylated derivative.

2. The reproducibility of the method was demonstrated by the consistent estimates obtained for the concentrations of noradrenaline, dopamine and 3-methoxytyramine in whole rat brain. Adrenaline and metanephrine were not detected. The concentration of normetanephrine in rat brain was at the limit of detection of the method.

3. Although the estimation for the levels of endogenous amines in whole rat brain were consistent, the recoveries of exogenous amines taken through the procedure were low and very variable. Control experiments demonstrated that the exogenous amines were lost at the perchloric acid extraction stage of the procedure.