流动注射化学发光分析法测定蒽醌类药物

基于蒽醌类药物在碱性条件下对高碘酸钾-鲁米诺化学发光体系的化学发光信号有强烈的抑制作用这一现象,结合流动注射技术建立了一种直接测定蒽醌类药物的流动注射化学发光分析新方法。该方法测定大黄素的线性范围为1.0×10-8—3.0×10-7g/mL,检出限为2×10-9g/mL;测定大黄酸的线性范围为7.0×10-8—3.0×10-6g/mL,检出限为2×10-8g/mL;测定大黄素甲醚的线性范围为1.0×10-9—5.0×10-8g/mL,检出限为3×10-10g/mL。该方法操作简单快速、灵敏度高,可用于样品中蒽醌类药物含量的准确测定。     

Effect of ultrasound on binding interaction between emodin and micellar casein and its microencapsulation at various temperatures

Emodin is a bioactive compound with strong anti-inflammatory and antioxidant properties. Micellar casein is casein concentrates close to the native state of casein micelles. The interaction of emodin and micellar casein under heat treatment in the absence and presence of ultrasound was investigated, and the properties of microencapsulated emodin in micellar casein were compared. Fluorescence experiments proved that the major interaction between emodin and micellar casein was through hydrophobic forces under heat treatment in the absence and presence of ultrasound. However, ΔH, ΔS and ΔG of emodin-casein complexation without sonication were higher than those with sonication, in contradiction to binding constants. The particle sizes of emodin-casein complexes in the presence of ultrasound were smaller than those without sonication, while the specific surface area showed an opposite trend. As to encapsulation, emodin-casein capsules under heat-sonication treatment showed higher antioxidant properties than those of heat treatment alone under similar experimental conditions. Interestingly, micellar casein-emodin encapsulation in the presence of ultrasound showed a lower release rate of emodin in gastrointestinal conditions than that without ultrasound at the emdoin concentration of 10 μmol per gram casein. Ultrasound has been shown to be a potential processing technology for customizing the release kinetics of bioactive compounds.     

Ultrasonic extraction and separation of anthraquinones from Rheum palmatum L

The ultrasonic nebulization extraction (UNE) was developed and applied to extract anthraquinones (emodin, aloe-emodin and rhein) from Rheum palmatum L. Several parameters of UNE, including type of extraction solvent, concentration of extraction solvent, volume of extraction solvent, extraction time and ultrasonic power, were studied and the optimized parameters were selected. The operation conditions of micellar electrokinetic capillary chromatography (MEKC) were also studied. Under the selected conditions, contents of emodin, aloe-emodin and rhein obtained from different cultivated areas of R. palmatum L. were 1.08–2.04 mg/g, 0.65–1.16 mg/g and 0.70–2.90 mg/g, respectively. The relative standard deviations (RSDs) for emodin, aloe-emodin and rhein were 1.3–2.4%, 1.9–4.7% and 1.3–3.9%, respectively. Compared with maceration extraction (ME), reflux extraction (RE), stirring extraction (SE) and ultrasonic extraction (UE), the proposed method was more efficient, faster and easier to be operated and lower equipment costs and lower extraction temperature were required. The results indicated that UNE was a good alternative method for extracting anthraquinones from R. palmatum L. Compared with traditional extractions, the proposed extraction has a potential in on-line sampling, especially when the gas is used as the carrier of sample.     

Plumbagin,a Naturally Occurring Naphthoquinone: Its Isolation,Spectrophotometric Determination in Roots,Stems, and Leaves in Plumbago Europaea L.

A new method for isolation and spectrophotometric determination of plumbagin is presented. Plumbagin was isolated by thin layer chromatography (TLC) and column chromatography (CC) techniques, as an orange tinged yellow long crystalline substances. Plumbagin exhibits two absrop-tion maxima at 410 and 510 nm. Stability of the color, pK_a value, and the effect of pH were studied. Beer's law is obeyed over the range 0.9-45 ppm. The method is applied to the determination of plumbagin in roots, stems, and leaves of Plumbago europaea L. plant.     

Simultaneous determination of amlodipine besylate and rosuvastatin calcium in binary mixtures by voltammetric and chromatographic techniques

Voltammetric and liquid chromatographic (LC) methods have been developed for the simultaneous determination of amlodipine besylate (AML) and rosuvastatin calcium (ROS) for the first time. Detailed electrochemical behavior and simultaneous voltammetric determination of AML and ROS were investigated in detail using glassy carbon electrode (GCE). High-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were also developed for the comparison. Voltammetric method exhibited linear dynamic responses for the simultaneous assay of AML and ROS in the concentration range between 0.006 and 2.85 μg/mL and between 0.01 and 5.00 μg/mL, with detection limits of 0.001 and 0.003 μg/mL, respectively. On the other hand, LC methods presented a wider linearity range than that of the SWV method between 0.5 and 100 μg/mL with the detection limits of 0.011 and 0.027 μg/mL for AML and 0.034 and 0.042 μg/mL for ROS by UPLC and HPLC techniques, respectively.     

大黄酸及大黄素和牛血清白蛋白的相互作用

采用荧光猝灭和红外光谱方法考察了两种大黄蒽醌类化合物(大黄酸和大黄素)与模型蛋白牛血清白蛋白之间的相互作用.结果表明,大黄酸和大黄素主要通过静电作用与牛血清白蛋白形成基态化合物,从而使其内部荧光猝灭,并获得了二者相互作用的结合常数、结合位点数及大黄酸和大黄素与色氨酸结合的空间距离.金属离子对这两种大黄蒽醌类化合物与牛血...     

电感耦合等离子体原子发射光谱/质谱法在中药微量元素及形态分析中的应用

本文对近年来电感耦合等离子体原子发射光谱法（ICP－AES）和电感耦合等离子体质谱（ICP－MS）在中药微量元素及形态分析中的应用进行了评述，讨论了应用ICP－AES／MS技术测定中药微量元素样品处理和各种分析方法，引用文献58篇。微波消解可作为中药微量元素分析理想的样品处理方法；ICP－AES／MS及各种联用技术在中药微量元素含量及形态分析中将发挥越来越重要的作用。     

RP-HPLC测定罗勒中石吊兰素的含量

建立反相-高效液相色谱法(RP-HPLC)测定罗勒(Ocimum basilicumL.)中石吊兰素的含量。用Microsorb-M V 100-5C18(4.6mm×250mm,5μm)色谱柱,甲醇:1%醋酸=86:14(V/V)为流动相,流速为0.5mL/min,检测波长为335nm。石吊兰素浓度在0.27—32.4μg/mL范围内与峰面积线性关系良好(r=0.9999),方法平均回收率大于99%(n=9)。方法简单、可靠,可应用于罗勒植物中石吊兰素的含量测定。     

离子色谱-氢化物发生-原子荧光法测定含金尾矿中砷

研究了离子色谱-氢化物发生-原子荧光(IC-HG-AFS)联用测定金矿尾矿淋滤液中各种价态砷的方法。以(NH₄)₂HPO₄溶液(pH 6.00)为流动相,阴离子分离柱分离,原子荧光进行检测,As(Ⅲ)加标回收率在97%～107%、As(Ⅴ)在95%～109%之间,相对标准偏差小于4%。从测试结果和色谱分离图可以看出,该方法能够使As(Ⅲ),As(Ⅴ),MMA和DMA等四种形态的砷完全分离。检出限可达到As(Ⅲ)1.0 μg·L-1,As(Ⅴ)2.3 μg·L-1。该方法适用于金矿石、尾矿石淋出液及金矿周遍环境水体中不同价态砷和总砷的定性和定量测定。     

HPLC测定护肝宁片中的大黄素

用十八烷基键合硅胶色谱柱,以甲醇-水-磷酸(800:200:0.2)为流动相,流速为1.0mL/min,检测波长为222nm.柱温30℃。大黄素在3.31—52.96μg/mL范围内线性关系良好(r=0.9999),平均回收率为99.7%(RSD为0.81%,n=9)。本法能显著分离大黄素与大黄酚,准确度高、精密度好,可在护肝宁片复方制剂中可靠地分离测定大黄素的含量,可用于其质量控制。     

头孢噻肟酸的高效液相色谱法

本文建立了头孢噻肟酸的高效液相色谱法，结果表明，在0-1.0mg范围内，峰面积与头孢肟酸的质量呈良好的线性关系，相关系数为0.9994，对0.05mg/mL标准溶液连续平行测定7次，相对标准偏差为3.14%，加标回收率在97.5%-104.4%之间，用于实际样品测定，结果令人满意。     

高效液相色谱法测定祛痘类化妆品中的苯海拉明

建立了高效液相色谱法测定祛痘类化妆品中禁用组分苯海拉明的含量。采用Inertsil CN-3色谱柱,流动相为乙腈-水-三乙胺(50∶50∶0.5,用冰醋酸调节pH至6.5),检测波长258nm,流速1.0mL/min,柱温25℃。苯海拉明在0.05—2.00mg/mL内呈良好线性(r=1.0000),平均回收率103.2%(RSD=0.70%,n=6);方法检出限(S/N=3)为50μg/g。该法操作简便,准确可靠,稳定性好,可用于祛痘类化妆品中苯海拉明的检测。     

HPLC测定烟用香精中的香豆素和黄樟素

建立了高效液相色谱-二极管阵列检测法测定烟用香精中香豆素和黄樟素的方法,样品用乙醇振荡萃取,萃取液经0.45μm滤膜过滤后,直接进行高效液相色谱分析,检测波长为280nm。该法的精密度均在10%以内,香豆素的回收率在88.0%—104.1%之间,黄樟素回收率在85.0%—98.8%之间,检出限分别为0.51、0.13mg/kg。方法简便、快速、准确,可用于烟用香精中香豆素和黄樟素的测定。     

色谱方法在植物黄酮含量测定中的应用

综述了黄酮类化合物含量的色谱测定方法,包括薄层扫描法、高效液相色谱、超临界流体色谱等,旨在为黄酮类化合物的研究、开发、应用提供参考.     

近红外光谱法测定不同产地独活中蛇床子素和二氢欧山芹醇当归酸酯含量

应用近红外光谱技术建立对独活中蛇床子素和二氢欧山芹醇当归酸酯的快速检测方法。自不同产地采集97批样品,通过高效液相色谱法测定指标成分含量,并测定样品的近红外光谱图,由于光谱图间差异较小,需要进行光谱预处理,通过比较不同预处理方法的结果,选择最优模型参数,结合偏最小二乘法分别建立独活中蛇床子素和二氢欧山芹醇当归酸酯的定量分析模型。结果显示,预处理方法为一阶导数时,蛇床子素的模型处于最优化性能,模型的相关系数为0.941 3,RMSEP值为0.141;校正集相关系数为0.923 3,RMSEC值为0.163。不经预处理的二氢欧山芹醇当归酸酯模型处于最优化性能,模型的相关系数为0.857 4,RMSEP值为0.103;校正集相关系数为0.831 5,RMSEC值为0.112。研究表明,近红外光谱技术结合偏最小二乘法操作简便,测定方法快速、高效、无损,可以实现对独活中蛇床子素和二氢欧山芹醇当归酸酯的含量进行定量分析,为中药材的质量控制研究和含量测定提供了一种科学有效的方法,同时为近红外光谱技术发展中药实时分析开辟了一个新方法,对保证中药材质量稳定可控有重要意义。     

Direct Radioimmunoassay of Proinsulin and Insulin in Human Plasma by Chromatographic Technique

Specific method for direct radioimmunoassay of IRP and IRI separately in human plasma has been described. The method is used for extraction of total insulin and separation of IRP from IRI by paper chromatography to be assayed separately. The separation of the two components are indentified and confirmed by column chromatography, paper chromatography and U.V. spectral analysis in comparison with the standard compounds.

134 plasma samples of different cases were, investigated for determination of IRI, IRP and IRT, of which 39 normals, 16 normal obes, 21 juvinil diabetes, 18 adult oncet diabetes, 10 recent adult diabetes, 12 hypothroid and 18 bilharzial hepatosplenomegaly to evaluate the levels of the test in comparison with blood sugar concentration.     

Potential of using uric acid fluorescence in eye fluid for freshness assessment on Red Sea bream (Pagrus major)

Abstract

Fluorescence characteristics of uric acid in Red Sea bream (Pagrus major) eye fluid was explored as a potential rapid and simple assessment for fish freshness. To investigate this, eye fluid samples were collected during storage at 22?±?2?°C for standard uric acid measurements by high-performance liquid chromatography at 12?h intervals up until 36?h storage. Simultaneously, uric acid fluorescence spectroscopy measurements by fluorophotometer at 3?h intervals up until 36?h storage were made. High-performance liquid chromatography results showed the concentration of uric acid increased with storage time in the Red Sea bream eye fluid; changes similar to those observed in Japanese dace eye fluid, only differing in concentration and rate of accumulation. The fluorescence signals of uric acid in Red Sea bream eye fluid increased with storage time, which the high-performance liquid chromatography results confirmed. To further explore this, uric acid fluorescence signals were plotted against a standard fish freshness indicator “K value”, which is calculated from the concentration of adenosine triphosphate and its breakdown products using paper electrophoresis method. A good exponential relationship between these two parameters (determination coefficient of 0.94). A high linear correlation between the predicted K value from the uric acid fluorescence signals and the measured K value (determination coefficient of 0.94 and root mean square error of prediction of 6.37%) indicate uric acid fluorescence characteristics in fish eye fluid has a high potential to be employed as a new, fast and simple method to assess fish freshness.     

气相色谱法测定蔬菜中的13种农药残留量

建立了快速、简便测定蔬菜中的13种农药残留的方法。样品用乙腈∶乙酸=1000∶1(V/V)溶液提取,QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)方法净化,采用气相色谱法测定。13种有机氯农药加标回收率为70.0%—105.1%,该方法具有回收率高、样品处理快速、溶剂使用量少等优点,能够应用于蔬菜中农药残留量的快速检测。     

Near-infrared spectroscopy as a rapid tool for water content analysis in the partial oxidation of ethanol

Abstract

The oxidation of ethanol to acetaldehyde was previously investigated in a continuous flow bench scale reactor using a zirconium-oxide-supported vanadium catalyst. Products were analyzed by near-infrared spectroscopy, a fast and accurate tool for the determination of water, ethanol, and acetaldehyde content. Water content was calibrated by Karl Fischer titration while gas chromatography was used to calibrate ethanol and acetaldehyde contents. Near-infrared spectroscopy is a fast, cost-effective method for the determination of water, ethanol, and acetaldehyde products from partial ethanol oxidation.     

同步荧光法测定食品中维生素B1

本文研究了食品中维生素Ｂ１的同步荧光法测定条件，采用氯化钾－乙醇作柱层析洗脱液，碱性介质中氧化后立即调为中性，并加入表面活性剂ＯＰ对体系增稳增敏，取代丁醇萃取，经济方便，用于几种粮食样品的测定，结果满意。