高效液相色谱法测定牛膝颗粒中5-羟甲基糠醛和蜕皮甾酮的含量

提出了高效液相色谱法同时测定牛膝配方颗粒中5-羟甲基糠醛和蜕皮甾酮的含量的方法。采用SHIMADZU shim-pack VP-ODS(4.6mm×250mm,4.6μm)柱;用两种不同配比的乙腈和水混合溶液作为流动相,梯度洗脱;检测波长为279nm(5-羟甲基糠醛)和245nm(蜕皮甾酮)。5-羟甲基糠醛和蜕皮甾酮的质量浓度分别在0.390～100mg.L-1和3.125～100mg.L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)分别为1.95,2.01ng。5-羟甲基糠醛和蜕皮甾酮的平均回收率分别为99.7%,99.1%;相对标准偏差(n=5)分别为0.80%,0.67%。     

Wetting Kinetics for a Single Detergent Granule

A technique for investigating the rate of wetting of a detergent granule has been developed. The evolution with respect to time of the meridional profile of the granule/water meniscus system is recorded using a high speed video camera. Glass spheres of different hydrophilicity were used to calibrate the system. A real detergent granule (LAS) was shown to give wetting behavior intermediate to those shown by the calibrants. In all cases the characteristic time for the wetting process was of the order 10 milliseconds. The protocol developed seems likely to be applicable to powder systems having medium particle size. It might thus be useful for the study of wetting rates in powdered food systems such as soup powders and building materials such as sand.     

Simultaneous quantification of twelve active components in Yiqing granule by ultra-performance liquid chromatography: application to quality control study

An ultra‐performance liquid chromatography (UPLC) method coupled with photodiode array (PDA) detection has been developed and validated for simultaneous quantification of 12 active components (berberine, palmatine, jatrorrhizine, aloe‐emodin, rhein, emodin, chrysophanol, physcion, baicalin, baicalein, wogonoside and wogonin) in Yiqing granule. Optimum separation were achieved on a C₁₈ column (50 × 2.1 mm i.d., 1.7 µm particle) through a 7.5 min gradient delivery of a mixture of A (acetonitrile) and B (0.1% aqueous phosphoric acid containing 1.8 mmol/L sodium dodecyl sulfonate and 10% acetonitrile, v/v) at a flow rate of 0.3 mL/min at 30°C. Because of the different UV characteristics of these components, three detection wavelengths were used for quantitative analysis. All of the analytes showed good linearity (r of >0.999). The method was validated for repeatability, precision, stability, accuracy and selectivity. The validated method was applied to quality control of Yiqing granule from different production batches. Copyright © 2010 John Wiley & Sons, Ltd.     

Identification of chemical constituents and rat metabolites of Kangxianling granule by HPLC‐Q‐TOF‐MS/MS

A high‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass tandem mass spectrometry method was established to characterize the chemical constituents of Kangxianling granule (KXL), a traditional Chinese medicine formula, and the metabolic profile in rat urine and plasma after oral administration of KXL. A total of 27 compounds in KXL extract and 13 prototype compounds with 12 metabolites in rat urine and plasma were identified. Among the 27 detected compounds, 15 were identified by comparing the retention time and MS data with that of reference compounds and the other 12 compounds were tentatively assigned based on the MS data and reference literature. The main prototype components absorbed in rat were amygdalin, salvianolic acid B, tanshinones and anthraquinones. Hydroxylation, glucuronidation and sulfation were the principal metabolic pathways in rat. The results revealed that the 25 compounds identified in rat urine and plasma were the potential active ingredients of KXL, which provides helpful chemical information for further study of the pharmacology mechanism of KXL. Copyright © 2015 John Wiley & Sons, Ltd.     

WET-GRANULATION RESEARCH WITH APPLICATION TO SCALE-UP

Summary Granulation is a unit operation by which larger granules are produced from fine, powdery particles to improve appearance, flow properties and mixedness, reduce dustiness and, in general, produce engineered particles with superior attributes. Agglomeration in wet granulation is achieved by introducing a “binder” fluid onto a shearing mass of fine powders. This paper gives a general overview of the process with emphasis on a simplified granulation model based on a dimensionless parameter containing inertia and viscous dissipation energies between colliding particles: the so-celled Stokes number. The model incorporates most common features of all granulation devices (mixers) used in the pharmaceutical industry.Also described in the paper is a computer simulation that captures the movement of flowing powder in an ideal mixer-granu/ator with constant shear rate. A fraction of the total number of particles is wet (covered by binder and there-fore “sticky”) while the rest of the particles are dry. The numerical simulation depicts two distinct regimes of agglomeration found in a typical granulator: granule growth and subsequent breakup. During granule growth-simulations, final granule size and shape distributions are obtained by analyzing the size and shape of formed granules using a pattern-recognition technique. A second kind of simulation, also using rapid granular flow modeling, follows the rotation and deformation of an “agglomerate” held together by a liquid binder. Results from these simulations yield critical values of the Stokes number. Below the cdticel value, the agglomerates are stable and only rotate in response to shear while above the critical value they break into two or more pieces. At the critical value, they attain a steady elongated shape. Using values of the critical Stokes number, the model predicts the size of formed granules.The existence of the critical state in which granules attain a characteristic elongated shape is used to measure shear forces in a granulator by employing calibrated “test” particles of known strength. This knowledge is employed in granulation scale-up to determine a kinematic rule that conserves stresses in the small and the large-scale machines. It was found that conserving the magnitude of internal stresses in the moving powder yields granules with similar attributes in granulators of different size.     

激光驱动高速金属颗粒与气体相互作用

采用激光驱动技术模拟高速运动金属颗粒与气体相互作用过程,研究高速气固两相流输运过程。采用驱动靶优化设计、激光参数调节等方法对颗粒加速过程进行控制,利用高时空分辨率、高精度瞬态实验诊断技术获取高速颗粒瞬态物理图像。通过求解三维雷诺平均Navier-Stokes方程和刚体飞行六自由度动力学方程数值模拟高速单颗粒与气体混合过程,方程采用高斯−赛德尔隐式方法进行时间推进求解。研究表明,激光驱动方法能够有效地发射金属颗粒,阴影照相技术能够有效获取高速颗粒物理图像。数值模拟给出了高速颗粒与气体作用的流场参数。     

Modeling Ca-Polyanion Crosslinking in Secretory Networks. Assessment of Charge Density and Bond Affinity in Polyanionic Secretory Networks

Materials released by secretory cells are stored inside intracellular membrane-bound vesicles. These moieties are not freely diffusible in the vesicle but remain immobilized in a Ca²⁺-crosslinked condensed-phase polyanionic polymer matrix. During exocytosis a Na⁺/Ca²⁺ ion exchange process triggers a volume phase transition resulting in massive swelling and release of the materials to the extracellular space. Here we formulate a simple model to assess Ca²⁺-ion binding from the swelling kinetics of polymer networks. We found the diffusivity of the networks (D) exhibits a power-law dependency on the Ca²⁺ concentration where D ∝ [Ca²⁺]^−2/3. The model yields an estimate of charge density and ionic affinity of the polymer chains. Studies of post-exocytic swelling kinetics in airway mucin granules, mast cell granules and granules from the microalga (Phaeocystis globosa) were used to validate predictions from our model. These results suggest that independent of the cell type, from animal to plant cells, a single polyelectrolyte interaction mechanism appear to be responsible for product release in exocytosis.     

Three Diverse Granule Preparation Methods for Proteomic Analysis of Mature Rice (Oryza sativa L.) Starch Grain

Starch is the primary form of reserve carbohydrate storage in plants. Rice (Oryza sativa L.) is a monocot whose reserve starch is organized into compounded structures within the amyloplast, rather than a simple starch grain (SG). The mechanism governing the assembly of the compound SG from polyhedral granules in apposition, however, remains unknown. To further characterize the proteome associated with these compounded structures, three distinct methods of starch granule preparation (dispersion, microsieve, and flotation) were performed. Phase separation of peptides (aqueous trypsin-shaving and isopropanol solubilization of residual peptides) isolated starch granule-associated proteins (SGAPs) from the distal proteome of the amyloplast and the proximal ‘amylome’ (the amyloplastic proteome), respectively. The term ‘distal proteome’ refers to SGAPs loosely tethered to the amyloplast, ones that can be rapidly proteolyzed, while proximal SGAPs are those found closer to the remnant amyloplast membrane fragments, perhaps embedded therein—ones that need isopropanol solvent to be removed from the mature organelle surface. These two rice starch-associated peptide samples were analyzed using nano-liquid chromatography–tandem mass spectrometry (Nano-HPLC-MS/MS). Known and novel proteins, as well as septum-like structure (SLS) proteins, in the mature rice SG were found. Data mining and gene ontology software were used to categorize these putative plastoskeletal components as a variety of structural elements, including actins, tubulins, tubulin-like proteins, and cementitious elements such as reticulata related-like (RER) proteins, tegument proteins, and lectins. Delineating the plastoskeletal proteome begins by understanding how each starch granule isolation procedure affects observed cytoplasmic and plastid proteins. The three methods described herein show how the technique used to isolate SGs differentially impacts the subsequent proteomic analysis and results obtained. It can thus be concluded that future investigations must make judicious decisions regarding the methodology used in extracting proteomic information from the compound starch granules being assessed, since different methods are shown to yield contrasting results herein. Data are available via ProteomeXchange with identifier PXD032314.     

抛光砖废料制备吸音材料

本文以微孔吸声结构原理为主要设计依据,以抛光砖废料制备的陶粒、澎胀水泥、粉煤灰以及造孔剂、防水剂等为主要原料,采用混凝土成型法成型,研究开发一种无有害成分的环保型吸声材料.通过试验分析了材料中胶凝材料和发泡剂的用量、厚度以及表面形态、背后空腔对材料吸声性能的影响.     

Analysis of chemical components in herbal formula Qi Bai Granule by UPLC-ESI-Q-TOF-MS

Qi Bai Granule (QBG), a traditional Chinese medicine formula for the treatment of idiopathic thrombocytopenic purpura, is composed of seven herbs. It is necessary to learn its chemical composition for quality control. In this study, a method for rapid separation and structural identification of the constituents in QBG was established by UPLC-ESI-Q-TOF-MS in negative and positive ion mode. As a result, 112 compounds, such as triterpenoids, flavonoids and monoterpenes were detected. Based on the retention times, accurate masses, fragment ions, related literatures, and/or authentic standards, 107 compounds were unambiguously identified or tentatively characterized. Additionally, 20% monarch, 50% minister, 5% assistant and 24% guide drugs of 112 compounds were detected, which on the whole was consistent with the compatibility of QBG. The results would provide a scientific basis for the quality control, quantitative analysis and further study in vivo or vitro of QBG.