金纳米微粒与盐酸氯丙嗪相互作用的共振Rayleigh散射光谱研究及其分析应用

在pH 1.8~3.3的酸性介质中,金纳米微粒本身有一定的共振瑞利散射(RRS)强度,但盐酸氯丙嗪本身的RRS强度十分微弱,当二者共存时,溶液的RRS强度显著增强并出现新的RRS光谱,在280~368 nm之间产生强烈的散射带,其最大散射波长位于368 nm,并在284、440、498 nm处有明显的散射峰。在一定条件下,盐酸氯丙嗪在0~0.08 mg/L范围内与ΔIRRS强度成正比,方法具有较高的灵敏度,对盐酸氯丙嗪的检出限(3σ)达到1.75μg/L。本文考察了反应体系的RRS光谱特征,研究了适宜的反应条件、影响因素及分析化学性质,研究了共存物质的影响,表明方法具有较好的选择性,据此发展了一种用金纳米微粒作RRS探针测定盐酸氯丙嗪的新方法。     

毛细管电泳法快速测定复方地芬诺酯片中的地芬诺酯和阿托品

建立了毛细管电泳高频电导法同时测定地芬诺酯和阿托品的方法。探讨了缓冲溶液、有机溶剂添加剂、分离电压和进样条件以及毛细管内径和长度等因素对分离检测的影响。在电泳介质为10.0mmol/L乳酸-15.0?H5OH、分离电压20.0kV的优化条件下,6min内即可实现地芬诺酯和阿托品的同时分离检测,线性范围分别为5.00~500和2.00~320mg/L;检出限分别为3.0和1.0mg/L。     

顶空气相色谱法测定盐酸托莫西汀中有机溶剂残留量的研究

建立了盐酸托莫西汀中有机溶剂残留量的顶空气相色谱分析方法.选用大口径HP-快速GC残留溶剂柱为分离柱,FID为检测器,外标法进行定量,并对顶空平衡温度、平衡时间、供试品溶液的制备方法对残留有机溶剂测定的影响进行了研究.甲醇、乙醚、正己烷、乙酸乙酯、四氢呋喃的线性范围分别为 0.41～8.10 μg/mL(r=0.9999)、0.15～3.00 μg/mL(r=0.9995)、0.20～4.01 μg/mL(r=0.9991)、0.32～6.35 μg/mL(r=0.9999)、0.36～7.11 μg/mL(r=0.9999);平均回收率范围96.30%～105.47%,精密度RSD(n=6)2.1%～3.7%;检出限分别为0.2、0.008、0.003、0.04、0.04 μg/mL.     

单层碳纳米管修饰电极上盐酸曲普利啶的电化学行为及其应用研究

应用循环伏安法研究了盐酸曲普利啶在碳纳米管修饰电极上的电化学行为.结果表明:在0.1 mol/L磷酸盐缓冲溶液(pH 6.9)中,盐酸曲普利啶产生一灵敏的氧化峰,其峰电位为0.81 V(vs.Ag/AgCl),峰电流与盐酸曲普利啶在1.0×10-6～1.3×10-4 mol/L浓度范围内呈线性关系,检出限为5.0×10-7mol/L,已用于片剂中盐酸曲普利啶的测定.     

Preparation of Ultrafine Colloidal Gold Particles using a Bioactive Molecule

Synthesis of nanometer-sized particles with new physical properties is an area of tremendous interest. In metal particles, the changes in size modify the electron density in the particles, which shifts the plasmon band. The most significant size effects occur when the particles are ultrafine (size is <10 nm). Thus the synthesis of ultrafine metal particles is enormously important to exploit their unique and selective application. Here we report a novel method for the synthesis of ultrafine gold particles in the size range of 0.5–3 nm using dopamine hydrochloride (dhc), an important neurotransmitter. This is the first time where such an important bioactive molecule like dhc has been used as a reagent for the transformation of Au(III) to Au(0). The synthesis is carried out, for the first time, either in simple aqueous or in a nonionic micellar (for example Triton X-100 (TX-100)) medium. The gold sol has a beautiful yellow–brown color showing _max at 470 nm. The appearance of the absorption peak at substantially shorter wavelength (usually gold sol absorbs at 520 nm) indicates that the particles are very small. The method discussed here is very simple, reproducible and does not involve any reagent, which contains 'P' or 'S' atoms. Also in this case no polymer or dendrimer or thiol-related stabilizer is used. The effects of different parameters (such as the presence or absence of O₂, temperature, TX-100 concentration and dhc concentration) on the formation of ultrafine gold particles are discussed. The effects of 3-mercapto propionic acid and pyridine on the ultrafine gold sol are also studied and compared with those on photochemically prepared gold sol. It is observed that 3-mercapto propionic acid dampens the plasmon absorption at 470 nm of ultrafine gold particles. Pyridine, on the other hand, has no effect on the particles.     

Alkynylation of Cotarnine Hydrochloride by Ag(I) Acetylenides

1-Organoacetylene derivatives were prepared by reaction of cotarnine hydrochloride with silver organoacetylenides with brief heating in acetonitrile. The structure of one of these, 1-(3-hydroxypropyn-1-yl)-2-methyl-6,7-methylenedioxy-8-methoxy-1,2,3,4-tetrahydroisoquinoline, wasproved by an X-ray structure analysis.     

Fluoxetine Hydrochloride的NMR数据解析

由美国Lilly公司开发的第二代抗抑郁症药物盐酸氟西汀（Fluoxetine hydrochloride），属于选择性5-羟色胺再摄取抑制剂（SSRI），除了用于治疗各类抑郁症，包括轻性或重性抑郁症，尤宜用于老年性抑郁症之外，对于强迫症、惊恐发作、贪食症、经前期焦虑等亦有很好疗效. Fluoxetine hydrochloride是一种双环化合物，与传统的三环类、杂环类或单胺氧化酶抑制剂抗抑郁药相比，具有疗效好、不良反应轻而少，安全性高、耐受性好等特点，目前已作为一线的抗抑郁药得到广泛应用. 本文对Fluoxetine hydrochloride进行了¹H NMR和¹³C NMR检测，并通过DEPT和¹H-¹H COSY、HMBC、HSQC等2D NMR技术对其¹H NMR和¹³C NMR数据进行了较为详细的解析和比文献[1]更为全面的NMR归属，为以后的分析鉴定提供更完善的依据.     

同时测定三辛胺和三辛胺盐酸盐的双波长分光光度法

提出了利用双波长分光光度法测定三辛胺（ＴＯＡ）及三辛胺盐酸盐（ＴＯＡ·ＨＣｌ）的一种新方法，即ＴＯＡ和ＴＯＡ·ＨＣｌ在ＣＣｌ４溶液中与Ｉ２生成电荷转移化合物，其最大吸收波长分别为２９３ｎｍ和２６３ｎｍ，两组分同时存在时可利用吸光度的加和性得联立方程，分别求出两组分的含量。ＴＯＡ含量在０～３５ｍｇ／Ｌ，ＴＯＡ·ＨＣｌ含量在０～３１ｍｇ／Ｌ范围内符合比耳定律。该法简便快速，方法的回收率为９５．５％～１０４．６％，能够满足分析的需要     

An efficient synthesis of 1-H indazoles

The reaction of substituted salicyaldehydes with hydrazine hydrochloride under different conditions gave the corresponding 1-H indazoles. However, the reaction of benzaldehydes with hydrazine hydrate under the same conditions yielded only hydrazones.     

复方氯丙那林质量检控的近红外光谱快速分析

基于近红外光纤漫反射技术,利用偏最小二乘法分别建立了复方氯丙那林胶囊的三种药效成分盐酸氯丙那林、盐酸溴己新和盐酸去氯羟嗪的快速同时测定方法。所建立的盐酸氯丙那林、盐酸溴己新和盐酸去氯羟嗪的定量分析多元校正模型的相关系数分别为99.7%、99.4%和99.0%,校正集的均方根残差分别为0.028、0.145和0.250,预测均方根误差分别为0.055、0.120和0.210。由于该方法是在不经任何预处理的情况下的光纤快速同时分析,因此可用于复方氯丙那林的过程质量控制。