LC–MS/MS method for simultaneous determination of flavonoids and physalins in rat plasma: Application to pharmacokinetic study after oral administration of Physalis alkekengi var. franchetii (Chinese lantern) extract

A rapid and sensitive liquid chromatography with tandem mass spectrometry (LC‐MS/MS) method was developed and validated for the simultaneous determination of luteolin, luteolin‐7‐O ‐β ‐D‐glucopyranoside, physalin A, physalin D and physalin L in rat plasma. Scutellarein and dexamethasone were used as the internal standards (IS). Plasma samples were prepared by liquid‐liquid extraction with ethyl acetate. The five constituents were separated on an Acquity UPLC BEH C₁₈ column (100 mm × 2.1 mm, 1.7 μm). A gradient elution procedure was used with acetonitrile (A)‐0.1% aqueous formic acid (B). Mass spectrometric detection was performed in negative ion multiple reaction monitoring mode with an electrospray ionization (ESI) source. This method showed good linearity (r ² > 0.997) over a concentration range of 2.0–500 ng/mL with a lower limit of quantification of 2.0 ng/mL for all five compounds. The inter‐ and intra‐day accuracy ranged from 91.7 to 104%, and precisions (RSD) were <6.46% for all analytes. The extraction recoveries of all analytes were >85%. This validated method was successfully applied for the first time to the pharmacokinetic study of five ingredients after oral administration of 70% ethanol extract of Chinese lantern in rats.     

中药炮制机理研究的思路与方法——以咖啡豆的烘焙原理研究为例

中药炮制是中药学的特色和优势,也是最具我国自主知识产权的学科之一.中药炮制研究的核心是阐明中药炮制机理,这也是制约中药现代化的关键节点.目前大部分中药的炮制机理尚不明确,有待进行系统深入的研究.咖啡豆需要烘培后才可以制成饮料,这个高温烘培过程类似于中药的炮制过程.近年来,国内外专家对咖啡豆高温烘培过程化学成分变化及其机理进行了深入研究,各种新方法和新技术得到广泛应用,取得了系列研究成果,这些研究成果为中药炮制机理研究提供了多种新思路和新方法,也为中药炮制机理的研究和阐明提供了重要示范.     

Accelerated solvent extraction and pH‐zone‐refining counter‐current chromatographic purification of yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom

This study aimed to seek an efficient method to extract and purify yunaconitine and 8‐deacetylyunaconitine from Aconitum vilmorinianum Kom. by accelerated solvent extraction combined with pH‐zone‐refining counter‐current chromatography. The major extraction parameters for accelerated solvent extraction were optimized by an orthogonal test design L₉ (3)⁴. Then a separation and purification method was established using pH‐zone‐refining counter‐current chromatography with a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (5:5:2:8, v/v) with 10 mM triethylamine in the upper phase and 10 mM HCl in the lower phase. From 2 g crude extract, 224 mg of 8‐deacetylyunaconitine (I) and 841 mg of yunaconitine (II) were obtained with a purity of over 98.0%. The chemical structures were identified by ESI‐MS and ¹H and ¹³C NMR spectroscopy.     

Screening of aromatase inhibitors in traditional Chinese medicines by electrophoretically mediated microanalysis in a partially filled capillary

An electrophoretically mediated microanalysis method with partial filling technique was developed for screening aromatase inhibitors in traditional Chinese medicine. The in‐capillary enzymatic reaction was performed in 20 mM sodium phosphate buffer (pH 7.4), and sodium phosphate buffer (20 mM, pH 8.0) was used as a background electrolyte. A long plug of coenzyme reduced β‐nicotinamide adenine dinucleotide 2′‐phosphate hydrate dissolved in the reaction buffer was hydrodynamically injected into a fused silica capillary followed by the injection of reaction buffer, enzyme, and substrate solution. The reaction was initiated with a voltage of 5 kV applied to the capillary for 40 s. The voltage was turned off for 20 min to increase the product amount and again turned on at a constant voltage of 20 kV to separate all the components. Direct detection was performed at 260 nm. The enzyme activity was directly assayed by measuring the peak area of the produced β‐nicotinamide adenine dinucleotide phosphate and the decreased peak area indicated the aromatase inhibition. Using the Lineweaver–Burk equation, the Michaelis–Menten constant was calculated to be 50 ± 4.5 nM. The method was applied to the screening of aromatase inhibitors from 15 natural products. Seven compounds were found to have potent AR inhibitory activity.     

A new strategy based on cholesterol-functionalized iron oxide magnetic nanoparticles for determination of polycyclic aromatic hydrocarbons by high-performance liquid chromatography with cholesterol column

This study reported for the first time the use of cholesterol-functionalized magnetic nanoparticles (Fe₃O₄@SiO₂@Chol) for the determination of polycyclic aromatic hydrocarbons (PAHs) in traditional Chinese medicine samples (TCMs) by high performance liquid chromatography (HPLC) coupled with fluorescence detection. The method was efficient, environmentally friendly, and fast. The solvent consumption of the proposed column is only half of the conventional column but with higher efficiency. Influencing factors, including sorbent amount, desorption solvent, sample volume and extraction time, were investigated in detail. Under the optimum conditions, good linearity (R² > 0.991) was obtained over the range of 5–400 ng g⁻¹, with limits of detection (LOD) 0.75, 0.50, 1.0, 0.56, 0.60, 0.84 and 0.80 ng g⁻¹ for anthracene, fluoranthene, pyrene, chrysene, benzo[a]anthracene, benzo(b)fluoranthene and benzo(k)fluoranthene, respectively.     

On the difference in material structure and fatigue properties of nylon specimens produced by injection molding and selective laser sintering

This paper describes the influence of dynamic tension/compression loading on notched and unnotched nylon specimens fabricated by Injection Molding (IM) and Selective Laser Sintering (SLS). The main objective of this work is to analyze and describe the differences in material structure and fatigue properties of as-built nylon parts produced by IM and SLM from the same polyamide 12 powder. The differences in dimensional quality, density, surface roughness, crystal structure and crystallinity are systematically measured and linked to the mechanical fatigue properties. The fatigue properties of the unnotched SLS specimens are found to be equal to those of the unnotched IM specimens. The presence of pores in the sintered samples does not lead to rapid failure, and the microvoid coalescence failure mechanism is delayed. The notched specimens show more brittle failure and increased fatigue resistance which is caused by local notch-strengthening. The results enable improved understanding of the difference in material structure and fatigue behavior of selective laser sintered and injection molded polyamide.     

DNA aggregation and cleavage in CGE induced by high electric field in aqueous solution accompanying electrokinetic sample injection

The phenomenon of peak area decrease due to high injection voltage (V_inj, e.g. 10–30 kV, 200–600 V/cm in the 50 cm capillary) was found in the analysis of very dilute DNA fragments (<0.2 mg/L) by using high‐sensitive electrokinetic supercharging‐CGE. The possibility of DNA cleavage in aqueous solution was suggested, in addition to the aggregation phenomenon that is already known. The analysis of intentionally voltage‐affected fragments (at 200 V/cm) also showed decreased peak areas depending on the time of the voltage being applied. Computer simulation suggested that a high electric field (a few kV/cm or more) could be generated partly between the electrode and the capillary end during electrokinetic injection (EKI) process. After thorough experimental verification, it was found that the factors affecting the damage during EKI were the magnitude of electric field, the distance between tips of electrode and capillary (D_e/c), sample concentration and traveling time during EKI in sample vials. Furthermore, these factors are correlating with each other. A low conductivity of diluted sample would cause a high electric field (over a few hundred volts per centimeter), while the longer D_e/c results in a longer traveling time during EKI, which may cause a larger degree of damage (aggregation and cleavage) on the DNA fragments. As an important practical implication of this study, when the dilute DNA fragments (sub mg/L) are to be analyzed by CGE using EKI, injection voltage should be kept as low as possible.     

一种嵌入式软件逻辑覆盖测试方法研究

针对嵌入式软件测试覆盖率低的问题,本文提出了基于软件故障注入的逻辑覆盖测试方法,首先就嵌入式系统常用传感器建立故障模式库,设计了嵌入式软件故障注入系统;其次选取中间层作为故障注入点,研究基于VxWorks653嵌入式操作系统的故障注入实现方式,并通过分析故障信号在软件系统中的传播,提出优化测试用例的方法;最后通过实验验证了该方法可有效提高容错设计功能、冗余设计功能、故障检测功能测试的逻辑覆盖率;有助于提高嵌入式软件的可靠性。     

中国煤中溴的含量及分布

在测试分析中国27个省、直辖市和自治区的305个煤样中溴含量的基础上,从煤的不同成煤年代、不同变质程度以及不同聚煤区等方面分析和考查中国煤中溴的分布状况。结果表明,中国煤中溴的含量为0.12~69.66μg/g,因其对数值呈正态分布,故可用其几何平均值(7.04μg/g)表征中国煤中溴的含量,该值低于大多数其他国家煤中溴的平均含量,和日本煤中溴的平均值(7.10μg/g)较为接近。按煤中溴的平均值,中国13个省市小于5μg/g;9个省为5~15μg/g;5个省市高于15μg/g。根据煤的变质程度,中国煤中溴含量按照烟煤、无烟煤、褐煤、次烟煤顺序依次下降;根据成煤地质年代,按早石炭纪、新近纪、晚石炭纪、早二叠纪、中侏罗纪、晚三叠纪、早侏罗纪、晚侏罗纪、古近纪、中石炭纪依次下降;根据聚煤区,按西北、华北、华南、滇藏和东北聚煤区依次下降。中国煤中溴的分布受多种因素的影响,任何单一因素和其没有密切的相关性。