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Dietary Green Tea Extract and Antioxidants Improve Insulin Secretory Functions of Pancreatic β-Cells in Mild and Severe Experimental Rodent Model of Chronic Pancreatitis
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作者 Galande Sheethal Ranjeet K. Tokala +7 位作者 Pavan Pondugala Krishna Vemula Vijayalakshmi Venkatesan Pothani Suresh Surya Satyanarayana Singh Guduru Venkat Rao Duvvur Nageshwar Reddy Mitnala Sasikala 《Open Journal of Endocrine and Metabolic Diseases》 2024年第2期53-72,共20页
Chronic pancreatitis (CP) is a progressive inflammatory disorder of the pancreas. It is predominantly idiopathic (with an unknown cause) in India and mostly due to alcohol in the West. Diabetes that occur secondary to... Chronic pancreatitis (CP) is a progressive inflammatory disorder of the pancreas. It is predominantly idiopathic (with an unknown cause) in India and mostly due to alcohol in the West. Diabetes that occur secondary to chronic pancreatitis (T3c Diabetes) is often brittle, and is difficult to attain normoglycemia with conventional treatment requiring multiple doses of insulin. Mild and severe model of CP was induced in mice by repeated intraperitoneal injections of cerulein and L-arginine respectively with an intent to study islet dysfunction and develop therapeutic strategy in animal models of CP. Dietary intervention of epigallocatechin-3-gallate (EGCG) was tested in both the models of CP for its beneficial effects on insulin secretory functions. Pancreata collected upon euthanasia were used to study alterations in the morphology of pancreatic parenchyma and inflammation by staining with H&E and fibrotic changes by Masson’s trichrome and picrosirius staining. Insulin secretory functions of islets were evaluated to test the efficacy of the dietary intervention on β-cell functions. Intraperitoneal glucose tolerance test was performed to monitor the glucose homeostasis before and after the dietary intervention. Both the models resulted in CP with dispersed acini, inflammation and fibrosis. The loss of acini and extent of fibrosis was more in L-arginine model. 2-fold improvement in glucose-stimulated insulin secretory functions of islets was observed with 0.5% EGCG dietary intervention in cerulein model of CP and 1.6-fold in L-arginine model of CP. A further improvement in insulin secretion by 3.2-fold was observed with additional dietary supplements like N-acetyl cysteine, curcumin in combination with EGCG. Our results thus demonstrate and highlight the therapeutic potential of dietary green tea (EGCG) supplementation in reversing islet dysfunction and improving glucose homeostasis in experimental chronic pancreatitis in mice. 展开更多
关键词 Dietary Intervention C57BL6/J Mice Epigallocatechin-3-Gallate n-acetyl Cysteine CURCUMIN Chronic Pancreatitis ISLETS Glucose Stimulated Insulin Secretion
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Cytoprotective effects of amifostine,ascorbic acid and N-acetylcysteine against methotrexate-induced hepatotoxicity in rats 被引量:3
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作者 Sami Akbulut Hulya Elbe +5 位作者 Cengiz Eris Zumrut Dogan Gulten Toprak Emrah Otan Erman Erdemli Yusuf Turkoz 《World Journal of Gastroenterology》 SCIE CAS 2014年第29期10158-10165,共8页
AIM: To investigate the potential role of oxidative stress and the possible therapeutic effects of N-acetyl cysteine (NAC), amifostine (AMF) and ascorbic acid (ASC) in methotrexate (MTX)-induced hepatotoxicity.
关键词 METHOTREXATE AMIFOSTINE n-acetyl cysteine Ascorbic acid HEPATOTOXICITY Oxidative stress
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Simultaneous Determination of N-Acetyl Cysteine and Taurine by HPTLC Method in Active Pharmaceutical Ingredient and Pharmaceutical Dosage Form
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作者 A. R. Magesh Magharla Dasaratha Dhanaraju 《American Journal of Analytical Chemistry》 2017年第11期742-751,共10页
Specific, precise and sensitive TLC-Densitometric method was developed and validated for the simultaneous estimation of N-Acetyl cysteine and Taurine in active pharmaceutical ingredient and pharmaceutical dosage form.... Specific, precise and sensitive TLC-Densitometric method was developed and validated for the simultaneous estimation of N-Acetyl cysteine and Taurine in active pharmaceutical ingredient and pharmaceutical dosage form. An effective separation was achieved on pre-coated silica gel HPTLC plates by using n-butanol:acetic acid:water (8:0.5:1.5 v/v/v). The spots were scanned densitometrically at 295 nm. The RF values of N-Acetyl cysteine and Taurine were found to be 0.29 and 0.52, respectively. Calibration curves were linear in the range of 30 - 180 and 100 - 600 ng/band for N-Acetyl cysteine and Taurine, correspondingly with correlation coefficients of 0.999. The developed method was validated as per ICH guidelines. The limits of detection were 11.24 and 63.40 ng/spot for NAC and TAU respectively. The method developed was found to be precise and specific for the simultaneous analysis of N-Acetyl cysteine and Taurine in pure and tablet dosage form. 展开更多
关键词 High Performance Thin Layer CHROMATOGRAPHY n-acetyl CYSTEINE TAURINE Validation
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Reversal Effects of N-Acetyl Cysteine on <i>Moringa oleifera</i>Leaves-Induced Sub-Acute Hepatotoxicity in Wistar Albino Rats
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作者 Josephine N. Kasolo Agnes Namaganda +5 位作者 Godfrey S. Bbosa Haruna Muwonge Robert Lukande Joshua Nfambi Ivan Kimuli Isaac Okullo 《Neuroscience & Medicine》 2019年第4期385-397,共13页
Background: M. oleifera is a highly valued medicinal plant used widely from time immemorial to treat various ailments. However, with continued un-standardized use of the plant leaves, studies have reported organ toxic... Background: M. oleifera is a highly valued medicinal plant used widely from time immemorial to treat various ailments. However, with continued un-standardized use of the plant leaves, studies have reported organ toxicity to the liver, kidney and the heart. As communities continue to use M. oleifera leaves for its medicinal and nutritional values, there is need to find an antidote for its hepatotoxicity. Aim: The study established the reversal effect of N-Acetyl Cysteine (NAC) on M. oleifera aqueous leaf extract-induced hepatotoxicity in Wistar albino rats. Methods: Twenty-four (24) rats received a toxic dose (8.05 g/kg bwt) of M. oleifera leaf extract for 28 days to cause sub-acute hepatotoxicity. They were divided into 4 groups of 6 rats each. Group I received 1 ml normal (control group), Group II received 1000 ng/kg NAC, Group III received 1200 mg/kg NAC and Group IV received 1500 mg/kg NAC. Another group of 6 rats (Group V) received 0.75 mg/kg Paracetamol to cause hepatotoxicity. Group V (a positive control) received the prescribed clinical dose of 1200 mg/kg NAC which reverses the hepatotoxicity. All the NAC doses were given once a day intragastric for 7 days. On days: 1, 3 and 7 of receiving NAC, liver serum enzymes and bilirubin were measured. On day 7 the animals were sacrificed and liver tissue harvested for histopathology analysis. Results: A dose of 8.05 g/kg of M. oleifera leaf extract and 0.75 mg/kg Paracetamol were able to induce hepatotoxicity in Wister albino rats in 28 days. The M. oleifera extract induced hepatotoxic rats treated with NAC at doses of 1000 mg/kg, 1200 mg/kg and 1500 mg/kg, had a reduction in mean serum liver enzymes, plus reduced mean serum bilirubin levels. The liver histopathological analysis showed reduced inflammation after treatment with NAC for 3 and 7 days in the M. oleifera and paracetamol induced hepatotoxic rats. Conclusion: NAC can reverse M. oleifera leaf aqueous extract-induced sub-acute hepatotoxicity in Wistar Albino rats. 展开更多
关键词 M. oleifera Sub-Acute HEPATOTOXICITY n-acetyl Cysteine WISTAR ALBINO Rat
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First Application of Optically Active trans-1,2-Bis(2- aminophenyl)cyclopentane for Asymmetric Reaction: Enantioselective N-Acetylation of Secondary Alkyl Amines
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《Chinese Chemical Letters》 SCIE CAS CSCD 2001年第1期1-4,共4页
关键词 First Application of Optically Active trans-1 2-Bis ENANTIOSELECTIVE n-acetylation of Secondary Alkyl Amines
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Simple HPLC-Fluorescence Determination of Raspberry Ketone in Fragrance Mist after Pre-Column Derivatization with 4-Hydrazino-7-nitro-2,1,3-benzoxadiazole 被引量:1
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作者 Yasuhiko Higashi 《Journal of Analytical Sciences, Methods and Instrumentation》 2016年第2期44-49,共6页
Raspberry ketone {RK, 4-(4-hydroxyphenyl)butan-2-one} is a natural compound contained in raspberry, and is added to cosmetics for skin whitening. It is very important to measure the RK level in cosmetics for quality a... Raspberry ketone {RK, 4-(4-hydroxyphenyl)butan-2-one} is a natural compound contained in raspberry, and is added to cosmetics for skin whitening. It is very important to measure the RK level in cosmetics for quality assessment, since RK structurally resembles 4-(4-hydroxyphenyl)-2-butanol, which causes leukoderma on consumers’ skin. Here, we present a simple HPLC-fluorescence method for determination of RK in a fragrance mist by pre-column derivatization with 4-hydrazino-7-nitro-2,1,3-benzoxadiazole hydrazine (NBD-H), which reacts with the carbonyl group of RK. The NBD-RK derivative was eluted from a reversed-phase ODS column, and detected with excitation at 470 nm and emission at 550 nm. The retention time of NBD-RK derivative obtained by reaction with NBD-H at 80°C for 20 min was 10.3 min. The standard curve was linear in the range of 0.2 to 10 μg/mL, with a correlation coefficient (r<sup>2</sup>) value of 0.9980. The lower limit of detection was 0.018 μg/mL (absolute amount of 1.8 pmol). The coefficients of variation were less than 8.1%. The content of RK in fragrance mist (1.00 mL) was 1.18 ± 0.07 mg (range: 1.12 to 1.28 mg, n = 5). Recovery tests were satisfactory (83.9% ± 3.9%;range: 79.6 to 88.8%, n = 5). 展开更多
关键词 Raspberry Ketone High-Performance Liquid Chromatography 4-hydrazino-7-nitro-2 1 3-benzoxadiazole Derivatization Fluorescence
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Therapeutic potential of N-acetyl cysteine during COVID-19 epoch
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作者 Ajita Kapur Munish Sharma Geetanjali Sageena 《World Journal of Virology》 2022年第2期104-106,共3页
N-acetyl cysteine(NAC)is a promising drug for prophylaxis and treatment of coronavirus disease 2019(COVID-19)based on antioxidant and anti-inflammatory mechanisms.Further studies with cautious approach are needed to e... N-acetyl cysteine(NAC)is a promising drug for prophylaxis and treatment of coronavirus disease 2019(COVID-19)based on antioxidant and anti-inflammatory mechanisms.Further studies with cautious approach are needed to establish the benefits and risks before considering NAC as an adjuvant treatment for COVID-19. 展开更多
关键词 n-acetyl cysteine COVID-19 COAGULOPATHY Therapeutic potential PROPHYLAXIS TREATMENT
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Repurposing the antioxidant and anti-inflammatory agent N-acetyl cysteine for treating COVID-19
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作者 Josef Finsterer Fulvio A Scorza +1 位作者 Carla A Scorza Ana C Fiorini 《World Journal of Virology》 2022年第1期82-84,共3页
Although several considerations have been raised suggesting a beneficial effect of N-acetyl cysteine(NAC)for the treatment of severe acute respiratory syndrome coronavirus 2 infection,there is currently no clinical ev... Although several considerations have been raised suggesting a beneficial effect of N-acetyl cysteine(NAC)for the treatment of severe acute respiratory syndrome coronavirus 2 infection,there is currently no clinical evidence that NAC truly prevents coronavirus disease 2019(COVID-19),reduces the severity of the disease,or improves the outcome.Appropriately designed clinical trials are warranted to prove or disprove a therapeutic effect of NAC for COVID-19 patients. 展开更多
关键词 n-acetyl cysteine SARS-CoV-2 COVID-19 Reactive oxygen species CYTOKINES
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2-肼基-4,6-二甲基嘧啶的高效液相色谱分析 被引量:3
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作者 李锋 丛健 王敏 《化学试剂》 CAS CSCD 北大核心 2005年第2期99-100,共2页
用高效液相色谱外标法对 2- 肼基 - 4 ,6- 二甲基嘧啶进行定量分析 ,以V甲醇∶V水 =90∶10为流动相 ,采用Kromasil 10 0 5C18色谱柱和紫外检测器。方法标准偏差为 0 .0 5 3,变异系数为 0 . 0 2 4 % ,平均回收率为 99 .6 %。
关键词 2-肼基-4 6-二甲基嘧啶 嘧菌腙 高效液相色谱
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1-氨基-1-肼基-2,2-二硝基乙烯(AHDNE)的合成、晶体结构和理论计算 被引量:10
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作者 常春然 徐抗震 +4 位作者 宋纪蓉 严彪 马海霞 高红旭 赵凤起 《化学学报》 SCIE CAS CSCD 北大核心 2008年第12期1399-1404,共6页
利用1,1-二氨基-2,2-二硝基乙烯(FOX-7)和水合肼在水体系中合成了1-氨基-1-肼基-2,2-二硝基乙烯(AHDNE),并在甲醇溶液中培养出可用于X射线衍射的单晶.晶体属正交晶系,空间群为Pnma,晶胞参数为:a=0.6283(4)nm,b=0.7713(5)nm,c=1.2280(8)... 利用1,1-二氨基-2,2-二硝基乙烯(FOX-7)和水合肼在水体系中合成了1-氨基-1-肼基-2,2-二硝基乙烯(AHDNE),并在甲醇溶液中培养出可用于X射线衍射的单晶.晶体属正交晶系,空间群为Pnma,晶胞参数为:a=0.6283(4)nm,b=0.7713(5)nm,c=1.2280(8)nm,α=β=γ=90°,V=0.5950(7)nm3,Dc=1.821g/cm3,μ=0.171mm-1,F(000)=336,Z=4,R1=0.0489,wR2=0.1456.选取标题化合物的一个结构单元作为初始模型,运用Gaussian03程序,在6-311+G(d)的基组水平上,用HF,MP2以及B3LYP三种计算方法对标题化合物进行了几何全优化,并对其成键情况及自然键轨道(NBO)进行了分析. 展开更多
关键词 1-氨基-1-肼基-2 2-二硝基乙烯(AHDNE) 1 1-二氨基-2 2-二硝基乙烯(FOX-7) 水合肼 晶体结构 理论计算
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联氨基姜黄素脂质体纳米颗粒对乳腺癌细胞增殖、凋亡、侵袭和迁移的影响 被引量:3
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作者 任玉国 张凤梅 +2 位作者 王敏 田文霞 伦立民 《现代肿瘤医学》 CAS 2016年第1期16-18,共3页
目的:研究联氨基姜黄素脂质体纳米颗粒(HC-NPs)对乳腺癌细胞的抑制作用及其机制。方法:制备HC-NPs,培养人乳腺癌MDA-MB-231细胞。以对数生长期的细胞为研究对象。分成对照组和实验组,对照组及实验组分别予以脂质体纳米颗粒空载(NPs)、HC... 目的:研究联氨基姜黄素脂质体纳米颗粒(HC-NPs)对乳腺癌细胞的抑制作用及其机制。方法:制备HC-NPs,培养人乳腺癌MDA-MB-231细胞。以对数生长期的细胞为研究对象。分成对照组和实验组,对照组及实验组分别予以脂质体纳米颗粒空载(NPs)、HC-NPs处理。测定细胞生长抑制率、移行愈合率,并测定相关蛋白Cyclin D1、Bcl-2、Bax、Survivin、MMP-9、p-STAT3的表达情况。结果:HC-NPs处理人乳腺癌MDA-MB-231后,与NPs对照组相比,可明显抑制细胞的增殖,差异有统计学意义(P<0.05)。FCM法检测实验组凋亡率高于对照组,差异有统计学意义(P<0.05)。细胞周期测定有显著差异,P均<0.05。HC-NPs作用于人乳腺癌MDA-MB-231细胞24h后,细胞周期停滞在G_2期。Transwell法检测到HC-NPs处理后,测定侵袭迁移,与对照组比较,HC-NPs组侵袭迁移能力明显低于对照组(P均<0.05)。Western blotting法测定相关蛋白p-STAT3、Cyclin D1、Bcl-2、Survivin、MMP-9的表达情况,HC-NPs组明显降低且低于对照组,而Bax明显增高且高于对照组,总STAT3水平无明显差异。结论:HC-NPs对乳腺癌细胞的抑制作用机制与下调JAK/STAT信号通路有关。 展开更多
关键词 乳腺癌细胞 联氨基姜黄素脂质体纳米颗粒 抑制作用
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AHMT分光光度法测定软骨鱼类硫酸软骨素 被引量:4
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作者 刘坤 高华 《中国海洋药物》 CAS CSCD 2005年第4期21-23,共3页
建立一种测定硫酸软骨素(ChS)的新方法.本方法利用4-氨基-3-肼基-5-巯基-1,2,4,-三唑(AH-MT)与硫酸软骨素反应生成紫色的衍生物,即6-巯基-3-均三唑并[4,3-b]对称四嗪,在540nm波长处测定硫酸软骨素,浓度在0.1~1.0g·L-1范围内符合... 建立一种测定硫酸软骨素(ChS)的新方法.本方法利用4-氨基-3-肼基-5-巯基-1,2,4,-三唑(AH-MT)与硫酸软骨素反应生成紫色的衍生物,即6-巯基-3-均三唑并[4,3-b]对称四嗪,在540nm波长处测定硫酸软骨素,浓度在0.1~1.0g·L-1范围内符合朗伯比耳定律,该方法简单、快速,灵敏度高. 展开更多
关键词 硫酸软骨素 分光光度法 4-氨基-3-肼基-5-巯基-1 2 4-三唑
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含5-苯基2-呋喃环的3(2H)哒嗪酮类衍生物的合成与生物活性(I)(英文) 被引量:1
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作者 崔紫宁 梁志彬 +2 位作者 田芳 刘诗胤 闫晓静 《农药学学报》 CAS CSCD 北大核心 2014年第3期252-258,共7页
为探索新的农药先导化合物,经取代苯基呋喃甲酰氯与5-肼基-3(2H)哒嗪酮反应,得到15个未见文献报道的含呋喃环3(2H)哒嗪酮类化合物,其结构均通过了红外光谱、核磁共振氢谱和元素分析确认。初步生物活性测定结果表明,目标化合物具有良好... 为探索新的农药先导化合物,经取代苯基呋喃甲酰氯与5-肼基-3(2H)哒嗪酮反应,得到15个未见文献报道的含呋喃环3(2H)哒嗪酮类化合物,其结构均通过了红外光谱、核磁共振氢谱和元素分析确认。初步生物活性测定结果表明,目标化合物具有良好的杀菌活性,但杀虫活性较弱。其中化合物3k在50 mg/L时对灰霉病菌的抑制率为86.29%±1.51%,与对照药剂腐霉利相当。初步的构效关系研究结果显示,苯环上取代基的种类和位置对杀菌活性有重要影响。 展开更多
关键词 5-苯基2-呋喃 5-肼基-3(2H)哒嗪酮 酰肼 合成 杀虫活性 杀菌活性
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[Co(C_2H_6N_6S)]ClO_4·2H_2O的合成、表征与性能研究 被引量:2
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作者 王燕兰 盛涤伦 +3 位作者 朱雅红 马凤娥 陈利魁 杨斌 《含能材料》 EI CAS CSCD 北大核心 2009年第4期389-391,共3页
合成出一种新型激光敏感配合物起爆药二水合高氯酸(3-肼基-4-氨基-5-巯基-1,2,4-三唑)合钴(TACo),得率达71%;用元素分析、红外光谱等分析方法对其进行结构表征;测试了它的激光感度和部分爆炸性能,该化合物起爆药在915 nm激发波长下的50... 合成出一种新型激光敏感配合物起爆药二水合高氯酸(3-肼基-4-氨基-5-巯基-1,2,4-三唑)合钴(TACo),得率达71%;用元素分析、红外光谱等分析方法对其进行结构表征;测试了它的激光感度和部分爆炸性能,该化合物起爆药在915 nm激发波长下的50%激光起爆能量密度为39.85 J.cm-2。实验结果表明:合成过程中温度和原料粒度对反应影响较大。 展开更多
关键词 有机化学 二水合高氯酸(3-肼基-4-氨基-5-巯基-1 2 4-三唑)合钴(TACo) 起爆药 配合物 合成 表征
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溶菌酶与邻-{2-[α-(2-羟基-5-磺酸苯偶氮)-亚苄基]肼基}苯甲酸反应的分光光度研究 被引量:1
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作者 迟燕华 庄稼 +1 位作者 张晓林 李克安 《分析测试学报》 CAS CSCD 北大核心 2004年第3期61-63,共3页
采用分光光度法对溶菌酶(Lys)与邻_{2_[α_(2_羟基_5_磺酸苯偶氮 )_亚苄基]肼基}苯甲酸 (ZCN)反应体系进行了研究 ,配合物的最大吸收波长为560nm ,与试剂本身比较 ,吸收峰红移100nm。实验研究了在 pH4.36的酸性条件下温度、时间、离... 采用分光光度法对溶菌酶(Lys)与邻_{2_[α_(2_羟基_5_磺酸苯偶氮 )_亚苄基]肼基}苯甲酸 (ZCN)反应体系进行了研究 ,配合物的最大吸收波长为560nm ,与试剂本身比较 ,吸收峰红移100nm。实验研究了在 pH4.36的酸性条件下温度、时间、离子强度等对反应体系的影响 ;测定了反应的线性范围为0~16mg/L ;最低检出限2.49×10 -7mol/L ,ZCN与Lys最大结合数n=19 ,表观摩尔吸光系数ε=0.971×105L·cm -1·mol -1 ;离解度α=0.217 ;结合常数K=7.81×106等 ,并对该反应体系的机理进行了研究 ,同时测定了无机物质、生物物质和表面活性剂对反应体系的干扰情况 ,并建立了溶菌酶与ZCN的研究体系。 展开更多
关键词 溶菌酶 邻-{2-[α-(2-羟基-5-磺酸苯偶氮)-亚苄基]肼基}苯甲酸 分光光度法
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卷烟主流烟气中挥发性羰基化合物分析研究进展 被引量:4
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作者 王丽苹 任凤莲 谢慧玲 《广州化学》 CAS 2008年第2期72-79,共8页
挥发性羰基化合物是卷烟烟气中主要有害成分之一,在抽吸卷烟的过程中会不同程度地刺激人体的感觉器官和呼吸系统,长期吸入会对人体造成严重的危害。文章介绍了卷烟主流烟气中挥发性羰基化合物的形成机制和前提物,综述了羰基化合物的捕... 挥发性羰基化合物是卷烟烟气中主要有害成分之一,在抽吸卷烟的过程中会不同程度地刺激人体的感觉器官和呼吸系统,长期吸入会对人体造成严重的危害。文章介绍了卷烟主流烟气中挥发性羰基化合物的形成机制和前提物,综述了羰基化合物的捕集方法、衍生化和检测手段。 展开更多
关键词 卷烟 主流烟气 羰基化合物 2 4-二硝基苯肼 巯乙胺 N-甲基-4-肼-硝基苯并呋喃 丹磺酰肼
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2-苯亚甲基肼基苯甲酸-4-磺酸的合成研究 被引量:1
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作者 袁其亮 沈德隆 +2 位作者 刘会君 钱捷 付庆 《精细化工中间体》 CAS 2005年第1期58-59,65,共3页
以2-氨基苯甲酸-4-磺酸为原料,经过重氮化,还原反应生成-2-羧基苯肼-5-磺酸,再与苯甲醛缩合,合成2-苯亚甲基肼基苯甲酸-4-磺酸。反应总收率约 90%。产物结构经 H1NMR和MS表征。
关键词 2-苯亚甲基肼基苯甲酸-4-磺酸 2-羧基苯肼-5-磺酸 2-氨基苯甲酸-4-磺酸 合成
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4-氨基-3-肼基-5-巯基-1,2,4-三唑的合成及其对醛的检验 被引量:1
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作者 谭日红 《化学试剂》 CAS CSCD 北大核心 2005年第5期305-306,共2页
以硫脲和水合肼合成了可用于检验醛的试剂———4-氨基3-肼基-5-巯基-1,2,4-三唑(别名:紫醛),其结构通过红外光谱、核磁进行了确定。试验表明,紫醛对醛的检验敏感、专一、快速、操作简单。
关键词 4-氨基-3-肼基-5-巯基-1 2 4-三唑 合成 检验
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取代甲铜络合物的合成研究 被引量:3
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作者 袁其亮 沈德隆 +2 位作者 刘祥洪 卢鑫鑫 陆丽萍 《浙江工业大学学报》 CAS 2005年第3期337-340,共4页
以2-氨基-4-磺基苯甲酸为原料,经过重氮化、还原,与苯甲醛缩合,生成中间体2-苯亚甲基肼基-4-磺基苯甲酸,再与3-乙酰氨基-5-氨基-4-羟基苯磺酸的重氮盐反应,生成N-(2-羧基-5-磺基苯基)-N'-(5-磺基-2-羟基-3-氨基苯基)-C-苯基甲化合... 以2-氨基-4-磺基苯甲酸为原料,经过重氮化、还原,与苯甲醛缩合,生成中间体2-苯亚甲基肼基-4-磺基苯甲酸,再与3-乙酰氨基-5-氨基-4-羟基苯磺酸的重氮盐反应,生成N-(2-羧基-5-磺基苯基)-N'-(5-磺基-2-羟基-3-氨基苯基)-C-苯基甲化合物,经铜离子络合,水解,生成四啮甲1∶1铜络合物.产品经液相色谱分析,纯度98%以上,λmax=603nm,总收率约75%.中间体2-苯亚甲基肼基-4-磺基苯甲酸收率85%以上,结构经1HNMR和MS表征确认.该工艺操作简单,收率较高,已经实现工业化生产. 展开更多
关键词 2-苯亚甲基肼基-4-磺基苯甲酸 3-乙酰氨基一5一氨基一4一羟基苯磺酸 N-(2-羧基-5-磺基苯基)-N′-(5-碘基-2羟基-3-氨基苯基)-C-苯基甲臢 合成
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HPLC法测定硝呋太尔的4种中间体的含量和有关物质 被引量:2
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作者 孙国祥 邓海莹 李闫飞 《西北药学杂志》 CAS 2011年第5期334-337,共4页
目的建立硝呋太尔合成过程中4种中间体2-(甲硫基甲基)-氧杂环丙烷(MMOP),3-甲硫基-2-羟基-丙基肼(HMPL),N-氨基-5-甲硫基甲基-2-唾唑烷酮(AMOD)和5-硝基糠醛(5-NFA)的HPLC分析方法。方法MMOP和5-NFA以70mmol·L^-1磷酸... 目的建立硝呋太尔合成过程中4种中间体2-(甲硫基甲基)-氧杂环丙烷(MMOP),3-甲硫基-2-羟基-丙基肼(HMPL),N-氨基-5-甲硫基甲基-2-唾唑烷酮(AMOD)和5-硝基糠醛(5-NFA)的HPLC分析方法。方法MMOP和5-NFA以70mmol·L^-1磷酸氢二钠溶液-甲醇(85:15)为流动相,HMPL和AMOD以70mmol.L^-1磷酸氢二钠溶液-乙腈(97:3)为流动相,MMOP、HMPL和5-NFA以AgilentZORBAXSB-Phenyl柱(250mm×4.6mm,5μm)分析,AMOD以AgilentEclipseXDB-C8柱(150mm×4.6mm,5μm)测定,检测波长分别为210,205,205和312nm。结果MMOP、HMPL、AMOD和5-NFA分别在7.4~266.4,26.0~2600,38.0~3800和18.5~1850μg·mL^-1范围内,峰面积与质量浓度呈良好的线性关系,平均回收率分别为99.9%,99.8%,100.1%和100.1%。4种中间体在酸、碱、氧化、直火和光照条件下的破坏实验时主成分峰与各降解产物及有关物质峰均能很好地分离。结论该方法简单、准确、重复性好,可用于硝呋太尔4种中间体的质量控制。 展开更多
关键词 HPLC 2-(甲硫基甲基)-氧杂环丙烷(MMOP) 3-甲硫基-2-羟基-丙基肼(HMPL) N-氨基-5-甲硫基甲基-2-噁唑烷酮(AMOD) 5-硝基糠醛(5-NFA) 硝呋太尔 有关物质
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