Droplet counter-current chromatography of alkaloids. The influence of ph-gradients and ion-pair formation on the retention of alkaloids

The separation of the alkaloids strychnine, brucine, quinine, dihydroquinine, and berberine by using pH-gradients in Droplet Counter-Current Chromatography was studied. Gradients from pH 8-2.5 resulted in separation of the alkaloids mentioned. It was further concluded that the anions play an important role in the distribution of the alkaloids between the organic and aqueous phase. Based on these conclusions a solvent system is proposed consisting of a pH = 4 Mcllvaine buffer containing 1 M sodium perchlorate - methanol - chloroform (3:5:5), using the aqueous phase as mobile phase (ascending mode) for the separation of the alkaloids. By using a gradient with a decreasing concentration of the counterion, the retention time of the alkaloids can be reduced.     

High-performance liquid chromatographic analysis of cyclosporin G (Nva2-cyclosporine) in human blood.

A sensitive high-performance liquid chromatographic method for the analysis of the immunosuppressant cyclosporin G (OG 37-325, Nva2-cyclosporine, CsG) in whole blood has been developed. Sample preparation, employing cyclosporin A (CsA) as internal standard, involves organic extraction with methyl t-butyl ether under sequential acidic and basic conditions. Chromatography is performed using a 2 mm inside diameter x 25 cm column packed with 5 microns octyl (C8) material. An isocratic mobile phase comprised of acetonitrile:methanol:water, at a flow rate of 0.4 ml/min, is utilized. Separation is monitored at 230 nm. Data are also presented that demonstrate the use of CsG as an alternative internal standard to cyclosporin D for liquid chromatographic determinations of CsA.     

The purification and partial characterisation of two novel metalloproteinases from the venom of the West African carpet viper, Echis ocellatus.

Separation of previously uncharacterised Echis ocellatus venom by phenyl-Superose FPLC (Fast Liquid Protein Chromatography) yielded eight protein fractions. Three of these displayed high proteolytic activity when assayed by in vivo and in vitro assays (including enzyme linked immunosorbant assay), and were further separated using Superdex 75 and Mono-Q FPLC. This resulted in the purification of a non-haemorrhagic 24 kDa metalloproteinase (EoVMP1, pI 7.0), and a haemorrhagic 56 kDa metalloproteinase (EoVMP2, pI 5.5). Following tryptic digest, short amino acid sequences of EoVMP1 and EoVMP2 were obtained using Edman degradation. Both sequences displayed homology when aligned with existing snake venom metalloproteinases (SVMPs). The strong homology observed among previously well-characterised SVMPs suggests that principles governing the interaction of substrates and inhibitors are likely to be similar for EoVMP1, EoVMP2 and all members of the reprolysin family.     

芪参益气滴丸治疗慢性心力衰竭疗效观察

目的探讨芪参益气滴丸治疗慢性心力衰竭的临床效果。方法本院慢性心力衰竭患者80例被随机分为观察组和对照组。两组患者均给予抗心力衰竭常规治疗,对照组采用常规治疗,观察组在常规治疗基础上给予芪参益气滴丸治疗。两组疗程为3个月。治疗前后采用超声心动图对两组进行检查。结果观察组治疗后左室射血分数、每搏量和每分心排出量显著高于对照组,差异有统计学意义（P〈0．05）;观察组总有效率与对照组比较,差异有统计学意义（P〈0．05）。结论芪参益气滴丸能够显著提高慢性充血性心力衰竭患者心功能,改善临床症状和体征,临床效果显著。     

舟山眼镜蛇毒细胞毒素的分离纯化及其体外抗肿瘤活性

目的从眼镜蛇毒中分离纯化细胞毒素 F(CTX F)并鉴定其活性。方法应用凝胶过滤、离子交换柱色谱及疏水柱色谱等方法从舟山眼镜蛇毒中分离纯化CTX F ,以SRB法观察CTX F对体外培养癌细胞的杀伤作用。结果眼镜蛇毒粗毒经凝胶过滤获得 4个蛋白峰 ,将CTX所在第Ⅳ峰用阳离子交换柱色谱获A、B、C、D、E、F和G等7个组分 ,其中E、F和G具CTX活性 ,将F组分再经凝胶过滤和疏水色谱进一步纯化得不含磷酯酶A2 (PLA2 )的CTX纯品 ,暂定名为CTX F ,它对多种癌细胞株有杀伤作用。结论应用凝胶过滤、离子交换和疏水色谱等方法可从眼镜蛇毒中获得不含PLA2 的CTX ,其组分F有抗肿瘤活性     

消炎止痛膏质量控制方法研究

目的：建立消炎止痛膏有效的质量控制方法。方法：采用薄层色谱法鉴别血竭、冰片;运用高效液相色谱法测定血竭中的血竭素含量。结果：薄层色谱方法简便、专属性强、重复性好;含量测定结果准确,血竭素的平均回收率为98.07%（RSD=1.53%,n=6）;血竭素在0.1～0.6μg/mL范围内呈良好的线性。结论：本方法可有效控制消炎止痛膏的质量。     

定心丸质量标准研究

目的建立定心丸质量标准。方法采用薄层色谱法对定心丸中的甘草,当归,远志进行定性鉴别,并用高效液相色谱法对定心丸中黄芩苷的含量进行测定,色谱柱为C18柱（250mm×4.6mm,5μm）,流速为1.0mL·min^-1,流动相为乙腈-0.2%磷酸（28∶72）,检测波长为280nm。结果甘草,当归,远志薄层色谱分离良好,斑点清晰可见;黄芩苷含量在0.1934～1.1606μg内线性关系良好,平均加样回收率为101.45%（RSD=1.2%,n=6）,精密度RSD=1.4%。结论该方法结果准确、重复性好,可作为该制剂的质量控制方法。     

牛黄解毒丸(水丸)薄层色谱鉴别方法研究

目的:建立牛黄解毒丸(水丸)的大黄、冰片薄层色谱(TLC)鉴别方法。方法:对大黄、冰片进行薄层色谱鉴别。结果:薄层色谱斑点清晰,阴性对照无干扰。结论:所用方法简便,重现性好,可用于牛黄解毒丸(水丸)的质量控制。     

现代分析技术在中药毒理学中的地位和作用

目的探讨现代分析技术在中药毒理学研究中的地位和作用。方法对国内近十几年来相关文献进行整理、分析与归纳。结果紫外分光光度法（UV）、原子吸收光谱法（AAS）、荧光光谱法、高效液相色谱法（HPLC）、气相色谱法（GC）、高效液相色谱-质谱联用技术（HPLC-MS）、气相色谱-质谱联用技术（GC-MS）和分子生物学技术是目前中药毒理学研究中常用的分析技术,其中HPLC、GC-MS、HPLC-MS应用最广泛。结论现代分析技术在中药体内过程研究中发挥着重要作用,主要用于血液或肝、肾等重要组织中有毒物质的浓度测定;而且随着现代分析技术的发展和分析仪器的灵敏度的提高,必将促进中药毒理学的进一步发展。随着现代毒理学中新技术、新理论的建立与发现,现代分析技术必将在中药毒效动力学（TD）和毒代动力学（TK）研究中占据不可或缺的地位,发挥着不可替代的作用。     

Preparation and characterization of salt forms of enalapril

Selection of an optimal salt form of a drug candidate is a vital component of preformulation stage of drug development. In this study, six salts of enalapril--citrate, mesylate, tartrate, malate, besylate and tosylate--were prepared and characterized by Mass Spectroscopy, Differential Scanning Calorimetry, Thermogravimetric Analysis, Microscopy, Powder X-ray Diffraction, Karl Fischer Titration, High Performance Liquid Chromatography, Fourier-Transform Infra-red Spectroscopy and Head Space Gas Chromatography. All the six salts were subjected to a tiered screening involving five stages in the following order: crystallinity, hygroscopicity, solubility, stability and flow/compactability. Enalapril malate showed encouraging profile because of its lower hygroscopicity, higher solubility, good solid state stability, and better flow and compactability, in comparison to the marketed maleate salt.     

Hydroxypropylmethylcellulose (HPMC) as emulsifier for submicron emulsions: influence of molecular weight and substitution type on the droplet size after high-pressure homogenization.

Hydroxypropylmethylcellulose (HPMC) is a known emulsifier as well as a common viscosity enhancer in eye drops. Therefore, HPMC stabilized emulsions appear as interesting drug carriers for ophthalmic use and as a suitable treatment of dry eye syndrome. Since submicron emulsions are known to have an improved drug delivery, attempts were made to reduce the emulsion's droplet size by high-pressure homogenization. Droplet size was dependent on the homogenization pressure and the polymer content. Differences were found between emulsions stabilized with higher and lower molecular weight HPMC. Smaller droplet sizes were obtained with the shorter chained HPMC. No considerable influence of the substitution type was observed.     

Separation of morphine and its oxidation products by capillary zone electrophoresis

Separation of morphine and its oxidation products (10-S-hydroxymorphine, pseudomorphine and morphine N-oxide) by capillary zone electrophoresis in Tris-borate buffer in the presence of cyclodextrins was studied. Pyridoxine was used as an internal standard.     

Evaluation of metered dose inhaler spray velocities using phase Doppler anemometry (PDA)

Droplet velocity is an important parameter which can significantly influence inhalation drug delivery performance. Together with the droplet size, this parameter determines the efficiency of the deposition of MDI products at different sites within the lungs. In this study, Phase Doppler Anemometry (PDA) was used to investigate the instantaneous droplet velocity emitted from MDIs as well as the corresponding droplet size distribution. The nine commercial MDI products surveyed showed significantly different droplet velocities, indicating that droplet velocity could be used as a discriminating parameter for in vitro testing of MDI products. The droplet velocity for all tested MDI products decreased when the testing distance was increased from 3 cm to 6 cm from the front of mouthpiece, with CFC formulations showing a larger decrease than HFA formulations. The mean droplet diameters of the nine MDIs were also significantly different from one-another. Droplet size measurements made using PDA (a number-based technique) could not be directly compared to results obtained using laser light scattering measurements (a volume-based technique). This work demonstrates that PDA can provide unique information useful for characterizing MDI aerosol plumes and evaluating MDI drug delivery efficiency. PDA could also aid the evaluation of in vitro equivalence in support of formulation or manufacturing changes and in evaluation of abbreviated new drug applications (ANDAs) for MDIs.     

气相色谱法测定蛹油中α-亚麻酸乙酯的含量

目的：用气相色谱内标法测定蛹油α－亚麻酸乙酯制剂中α－亚麻酸乙酯的含量。方法：采用气相色谱法，DEGS为固定相，涂布浓度为10％，载体为Chromosorb W AW DMCS80-100目的气相柱。结果：平均回收率为97.87%，RSD为1.52%。结论：该法操作简便、准确、重现性、稳定性好，可作为蛹油α－亚麻酸乙酯的含量测定方法。     

高效逆流色谱研究进展——在天然产物有效成分分离方面的应用

本文简述了HSCCC近年来在天然产物有效成分分离方面的应用,介绍了双向逆流色谱、正交轴逆流色谱、pH-区带精制逆流色谱和HSCCC与MS联用技术。     

Identification, synthesis and quantification of process-related impurities in auraptene

Impurities in chemically synthesized auraptene, an active pharmaceutical ingredient (API), were detected by a gradient Reverse-Phase High-Performance Liquid Chromatography (RP-HPLC) method. Molecular weights and major product ions of these chemical compounds were determined by Liquid Chromatography/Triple Quadrupole (LC-MS/MS) analysis. Structural assignments were presumed as umbelliferone (Imp-I), (E)-6,7-dihydroxy-3,7-dimethyl-2-octene-umbelliferone (Imp-II), (E)-6,7-epoxy-3,7-dimethyl-2-octene-umbelliferone (Imp-III) and 4-methylauraptene (Imp-IV). The impurities were authentically synthesized, confirmed by Nuclear Magnetic Resonance spectroscopy (NMR) and Infrared spectroscopy (IR), and subsequently used as reference samples in routing HPLC system suitability testing for method specificity and detectability. Method specificity was further verified by forced degradation studies. The developed method was validated for characterization of impurities in synthesized auraptene according to the guidelines of the International Conference on Harmonization (ICH) in our laboratory.     

高速逆流色谱技术在植物活性成分分离与纯化中的应用

高速逆流色谱是一种连续液-液色谱技术,具有无固相载体、样品无需严格预处理等优点。本文就近年来高速逆流色谱在植物有效成分分离方面的应用作了简述。     

Aufteilung des Acetylcholins im Rattenhirn in drei Fraktionen und Versuch einer funktionellen Zuordnung

Ohne Zusammenfassung

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Separation of acetylcholine in the rat brain into three fractions and an Attemp of a functional classification

     

退白汤中当归、黄芪、丹参、首乌、补骨脂的TLC法鉴别

目的制定退白汤的TLC鉴别方法。方法采用TLC法对处方中当归、黄芪、丹参、首乌、补骨脂的有效成分阿魏酸、黄芪甲苷、原儿茶醛、大黄素、香豆素类、补骨脂素、异补骨脂素进行定性鉴别。结果各品种的薄层色谱特征明显,专属性强。结论该方法可以准确地进行定性鉴别,能有效地控制退白汤的质量。     

Alkaloids from Egyptian Papaver rhoeas

N-methylasimilobine was isolated as the major alkaloid from an Egyptian sample of P. RHOEAS L. Other alkaloids isolated from the same plant material were stylopine, coptisine, isocorydine and rhoeadine. Chromatography indicated the presence of at least nine other minor alkaloids.