近红外光谱法快速测定异烟肼片

目的研究近红外光谱法在异烟肼片快速测定中的应用。方法应用偏最小二乘法建立计算模型,通过方差分析法选择计算波长,主成分分析法选择验证集和训练集,交互验证法选择适当的计算因子数。结果应用所建立的偏最小二乘法模型,对9份异炯肼片测定异烟肼含量,与HPLC法相比,所测结果相对误差≤±0．8％,方法准确可靠。结论可将近红外光谱法应用于异烟肼的快速测定,在异烟肼生产中的过程控制和快速质量检测上有较大应用前景。     

用6,7-二氯喹啉-5,8-二酮的分光光度法测定异烟肼

异烟肼的含量测定有容量分析法、紫外、荧光、原子吸收和色谱等方法。英国药典(BP,1980年版)和美国药典(USP,1985年版)分别用溴量法和亚硝酸钠法,但这两种方法均不理想。本文采用异烟肼与6,7-二氯喹啉-5,8-二酮(DCQD)反应,生成有色化合物后进行分光光度法测定。该方法具有灵敏度、选择性和稳定性好等优点。标准溶液的制备:精密称取约50mg的标准异烟肼溶于水中,在100ml容量瓶中稀释至刻度,取这种溶液存一系列50ml容量瓶中制成20～250μg/ml的溶液,备用。样品溶液的制备:对纯品直接溶于水中配制成200μg/ml的溶液。对片剂、合成药的混     

异烟肼的灵敏比色测定法

目前测定异烟肼的碘滴定法或美国药典(十八版)测定片剂中异烟肼的方法既费时又麻烦。本文报导一个简便且灵敏度高的比色法。本法是基于异烟肼在硼砂的无水甲醇溶液中与7-氯-4-硝基苯并-2-氧杂-1,3-二氮杂茂相互作用,产生的橙色物可在467毫微米处测定其吸收值。反应方程为: 异烟肼在0.3～5微克/毫升的浓度范围内,符合Beer-Lambert定律。在90分钟内显色稳定。测定9个含2微克/毫升的异烟肼样品的重演性,其标准偏差为0.87%。如测定过程中有水存在则重演性不佳。用本法测定片剂和糖浆中的异烟肼,并与美国药典(十八版)的方法作了比较,结果     

盐酸小檗碱片中掺入物的检出和定性定量分析

目的用各种检测方法确定盐酸小檗碱片中人为掺入物的成分及掺入量。方法经TLC分离提取后,用核磁共振和质谱定性为异烟肼,再用异烟肼原料做TLC法、UV法、HPLC法对照实验。结果确证掺入物与异烟肼的色谱图和光谱图均一致。用UV法和HPLC法测定结果每片中异烟肼掺入量为14mg左右。结论测定结果与样品实际测定情况完全吻合。     

异烟肼介入凝胶体外抗结核作用及安全性评价

目的：观察异烟肼凝胶体外抗结核活性和支气管介入的安全性。方法：手工法，仪器法分别测定异烟肼、异烟肼凝胶的最小抑菌浓度和最小杀菌浓度及家兔经支气管介入的安全性。结果：异烟肼凝胶对H37RV标准株，牛型结核分枝杆菌MIC值均为1mg.L^-1，对草分枝杆菌MIC值为8mg.L^-1，对H37RV标准株，牛型结核分枝杆菌MBC值均为4mg.L^-1，对草分枝杆菌MBC值为16mg.L^-1，异烟肼凝胶与异烟肼单体MIC、MBC值差异无显著性；动物安全性试验阴性，结论：异烟肼凝胶具有与异烟肼单体相同的抗结核菌药效，卡波姆基质不影响异烟肼的抗菌活性；卡波姆基质异烟肼凝胶应用安全。     

吡啶及其衍生物的流动注射荧光分析

本文利用吡啶及其衍生物与过氧化氢的加热反应,建立了流动注射荧光分析法。吡啶及其衍生物在5～100ng范围内具有良好的线性关系(r=0.999).异烟肼、乙酰异烟肼和异烟酸在进样25ng时的相对标准偏差(n=10)平均为1.2%。异烟肼、乙酰异烟肼的检出限(S/N=3)为0.5ng,异烟酸的检出限为0.25ng.分析速度为30样/h。     

一阶导数光谱法测定复方异烟肼片中异烟肼的含量

复方异烟肼片是由异烟肼、维生素B_6及淀粉等辅料制成的片剂,其中异烟肼的含量测定采用溴酸钾法,操作繁琐且受测定条件的限制(18～25℃)。本文用一阶导数光谱法,不经分离,直接测定异烟肼的含量,其平均回收率为100.1%,变异系数为0.37%。该法操作简便,快速,不受测定时温度的限制。     

地方性甲状腺肿非病区人群碘代谢调查(摘要)

本调查以桐梓县元田乡7～14岁在校学生为对象作甲状腺检查,同时在当地儿童、成人中分别随机抽样测定尿碘(碱灰化法)、血清T4(蛋白竞争结合分析法)、T3(放射免疫树脂法)、TSH(放射免疫双抗体法)、甲状腺吸~(131)碘率(限制高碘饮食,用闪烁探头及FH—408定标器,口服~(131)碘2微居里后,于第3、6、24小时分别测定)。结果表明:一、元田乡7—14岁学生甲状腺肿大率14.2％,较为接近病区相应标准(20％)。二、成人及儿童尿碘均值都在正常低水平。其中40.3％的人群低70ug/克肌酐;26.     

气液色谱法测定联苯哒嗪和异烟肼中的肼

由于动物试验表明肼是一种诱变剂和致癌物,人们对药物中肼的存在十分关注,因此现在肼的测定已经延伸到肼苯哒嗪,肼苯哒嗪中肼的沾污发生于合成过程或由于药物降解。本文研究了一种测定肼苯哒嗪和异烟肼原料、单、复方片剂、注射剂和糖浆剂中肼的GLC法,该法基于肼与苯甲醛生成苄连氮,最低检测浓度为～0.0003％。     

甾体激素的比色分析 Ⅰ.△~(1,4)-3-酮基及△~4-3-酮基甾体激素与異烟肼的比色测定

本文对Δ~(1,4)-3-酮基激素(去氢皮质醇,去氢可的松)与异烟肼的反应条件进行了试验,生成腙的最大吸收峯在400毫微米波长,符合Beer定律。运用于片剂的测定与对照法比较,结果一致,但本法较简便,省时。对Δ~4-3-酮基的六种激素在Umberger方法基础上,设计了用比色计测定的方法,运用于各种制剂的测定,与对照法比较,结果一致。     

Interaction of norethindrone and isoniazid following their oral co-administration to the minipig

Following the oral co-administration of isonicotinic acid hydrazide and norethindrone to minipigs, the hydrazone of norethindrone was detected in plasma as its p-methoxybenzaldehyde derivative, using a high performance liquid chromatographic technique. The suspected precursor of the hydrazone of norethindrone was isonicotinyl hydrazone of norethindrone, a reaction product probably formed between norethindrone and isonicotinic acid hydrazide in the acid environment of the stomach. An in vitro liver metabolite of isonicotinyl hydrazone of norethindrone was isolated following derivatization with p-methoxybenzaldehyde and characterized by high resolution mass spectrometric and radiochemical techniques. The results demonstrated that the hydrazone of norethindrone is a metabolite of isonicotinyl hydrazone of norethindrone.     

Fullerene Isoniazid Conjugate – A Tuberculostat with Increased Lipophilicity: Synthesis and Evaluation of Antimycobacterial Activity

A fullerene–isoniazid conjugate has been synthesized by 1, 3 dipolar cycloaddition reaction of fullerene (C₆₀) with isonicotinic acid (4‐formyl‐benzylidene) hydrazide and N‐methylglycine. The identity and purity of the compound was confirmed by elemental analysis, ¹H NMR, ¹³C NMR and MALDI‐TOF mass spectral analysis. Stable water suspension, in which the particles of the synthesized conjugate were made to aggregate in nanosize, was successfully tested for antimycobacterial activity against Mycobacterium avium and strains of Mycobacterium tuberculosis– H₃₇Rv & H6/99 at concentration as low as 0.50 μg/mL.     

New hydrazide–hydrazones of isonicotinic acid: synthesis,lipophilicity and in vitro antimicrobial screening

This study describes the synthesis, lipophilicity and in vitro antimicrobial assays of 15 new hydrazide–hydrazones of isonicotinic acid. New derivatives were obtained on the basis of the condensation reaction of isonicotinic acid hydrazide with different aromatic aldehydes. The chemical structure of synthesized compounds was confirmed by spectral methods. Experimental lipophilicity of new isonicotinic acid derivatives was determined using reversed‐phase thin‐layer chromatography. All synthesized compounds were subjected to in vitro antimicrobial assays against reference strains of Gram‐positive bacteria, Gram‐negative bacteria and fungi belonging to Candida spp. Some of the synthesized hydrazide–hydrazones proved to be significant antibacterial compounds and more potent than commonly used chemotherapeutic agents.     

Indirect determination of N-acetyltransferase activity using ammonium metavanadate for evaluating isoniazide excretion with human urine

Optimum conditions for the analytical determination of isonicotinic acid hydrazide in urine using ammonium metavanadate are established. Anoninvasive method for the indirect determination of N-acetyltransferase activity in human hepatocytes that is based on measurement of the isoniazide fraction excreted with urine for 6 h is proposed. Translated from Khimiko-Farmatsevticheskii Zhurnal, Vol. 42, No. 8, pp. 49–53, August, 2008.     

抗结核药物的研究—N,N′-双酰肼及多酰肼类化合物

一、N,N′-双酰肼类化合物的一般制法系将酸制成酯,酯与水合肼作用生成酰肼,酰肼与酰氯于无水吡啶或无水乙腈中反应,即可制得。本文合成酰肼化合物一个,N,N′-双酰肼类化合物共六个,其中三个化合物经药理试验结果,无抗结核作用。二、多酰肼类化合物系采用酯与水合肼作用而得,其氨硫脲的衍生物可采用酰氯与氨硫脲反应而得。本文合成多酰肼及其氨硫脲类衍生物共六个(两个系已知的),其中四个化合物经药理试验结果,无抗结核作用。     

Discovery of N-pyridoyl-Δ2-pyrazolines as Hsp90 inhibitors

Hsp90, as a key molecular chaperone, plays an important role in modulating the activity of many cell signaling proteins and is an attractive target for anticancer therapeutics. Herein, we report the discovery of N-pyridoyl-Δ²-pyrazoline analogs as novel Hsp90 inhibitors by integrated approaches of drug design, organic synthesis, cell biology, and qualitative proteomic analysis. Novel chemical compounds were designed and optimized in the adenosine triphosphate-binding site of Hsp90; lead optimized compounds were found to have significant interactions with Asp93 and other amino acids crucial for Hsp90 inhibition. The designed compounds were synthesized by a two-step procedure; different aromatic aldehydes were reacted with various acetophenones to form substituted 1,3-diphenyl-prop-2-enones ( Ic–Io ), which upon reaction with isonicotinic acid hydrazide in the presence of glacial acetic acid form N-pyridoyl-Δ²-pyrazoline compounds ( PY1–PY13 ). Compounds PY3 , PY2 , and PY1 were identified as potential leads amongst the series, with promising anticancer activity against human breast cancer and melanoma cells, and the ability to inhibit Hsp90 similar to radicicol by drug-affinity responsive target stability proteomic analysis in a whole-cell assay.     

甾体激素的比色分析 Ⅰ.△1,4-3-酮基及△4-3-酮基甾体激素与異烟肼的比色测定

本文对Δ^1,4-3-酮基激素(去氢皮质醇,去氢可的松)与异烟肼的反应条件进行了试验,生成腙的最大吸收峯在400毫微米波长,符合Beer定律。运用于片剂的测定与对照法比较,结果一致,但本法较简便,省时。对Δ⁴-3-酮基的六种激素在Umberger方法基础上,设计了用比色计测定的方法,运用于各种制剂的测定,与对照法比较,结果一致。     

Chemical properties and immunotropic activity of the products from reaction of N-(6-methyl-2,4-dioxo-1,2,3,4-tetrahydro-5H-pyrimidinesulfone)-N′-isonicotinoylhydrazide with acids and bases in aqueous media

The effect of tautomerism on the structure of products from the reaction of N-(6-methyl-2,4-dioxo-1,2,3,4-tetrahydro-5H-pyrimidinesulfone)-N′-isonicotinoylhydrazide (kristafon) with acids (hydrochloric, phosphoric, acetic, oxalic, succinic, citric, hyaluronic) and bases [sodium hydroxide, triethanolamine, tris-(hydroxymethyl)aminomethane] in aqueous media has been studied using UV, IR, PMR, and ¹³C NMR spectroscopy techniques. The properties of kristafon are compared to those of analogous compounds containing pyridine (isonicotine hydrazide, sulfotolylisonicotine hydrazide) and pyrimidine [bis-p-(2,4-dioxo-6-methylpyrimidinyl-5-sulfonamino)-diphenylsulfone] fragments in acid–base media. It is shown that the immunotropic activity of kristafon phosphate and kristafon are improved in hyaluronic acid solution.     

砷的极谱分析法

砷的極譜分析法在文献上記載得不算少,但文献上所發表的数据却極不一致。 Kacirkova氏發現As (3 )在1NHCI中显二个極化波,它們的开始电压为-0.3及-0.6伏特(对飽和甘汞电極)。这二个極化波的高度在低濃度时是相等的,但当As (3 )濃度增加到1mM以上时,第一波的高度就不再增高。Lingane氏做了同样試驗,但加0.01％骨胶做極譜峰的抑制剂,这样所得二个極化波的开始电压为-0.4及-0.9伏     

Zur enzymatischen Oxidation aromatischer Acylhydrazide

Enzymatic Oxidation of Aromatic Acyl Hydrazides The enzymatic oxidation of benzoic acid hydrazide within pH 5–9 gives benzoic acid (main product) and N,N′-dibenzoylhydrazine. In this respect benzoic acid hydrazide differs from isonicotinic acid hydrazide, which yields four products (isonicotinic acid, diisonicotinoylhydrazine, isonicotinamide, N-isonicotinoyl-N′-isonicotinal-hydrazone). Experiments to hydroxylate isonicotinic acid hydrazide by enzymes were unsuccessful.