An efficient combination of supercritical fluid extraction and high-speed counter-current chromatography to extract and purify homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler

Supercritical fluid extraction (SFE) was used to extract homoisoflavonoids from Ophiopogon japonicus (Thunb.) Ker-Gawler. The optimization of parameters was carried out using an orthogonal test L-9 (3)(4) including pressure, temperature, dynamic extraction time and the amount of modifier. The process was then scaled up by 100 times with a preparative SFE system under the optimized conditions of 25 MPa, 55 degrees C, 4.0 h and 25% methanol as a modifier. Then crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/ACN/water (1.8:1.0:1.0:1.2:1.0 v/v). There three homoisoflavonoidal compounds including methylophiopogonanone A 6-aldehydo-isoophiopogonone A, and 6-formyl-isoophiopogonanone A, were successfully isolated and purified in one step. The collected fractions were analyzed by HPLC. In each operation, 140 mg crude extracts was separated and yielded 15.3 mg of methylophiopogonanone A (96.9% purity), 4.1 mg of 6-aldehydo-isoophiopogonone A (98.3% purity) and 13.5 mg of 6-formyl-isoophiopogonanone A (97.3% purity) respectively. The chemical structure of the three homoisoflavonoids are identified by means of ESI-MS and NMR analysis.

One step isolation and purification of liquiritigenin and isoliquiritigenin from Glycyrrhiza uralensis Risch using high-speed counter-current chromatography

High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale has been successfully applied to the separation of bioactive flavonoid compounds, liquiritigenin and isoliquiritigenin in one step from the crude extract of Glycyrrhiza uralensis Risch. The HSCCC was performed using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-acetonitrile-water (2:2:1:0.6:2, v/v). Yields of liquiritigenin (98.9% purity) and isoliquiritigenin (98.3% purity) obtained were 0.52% and 0.32%. Chemical structures of the purified liquiritigenin and isoliquiritigenin were identified by electrospray ionization-MS (ESI-MS) and NMR analysis. (c) 2005 Published by Elsevier B.V.

Separation of neutral compounds by high speed capillary electrochromatography

With using short capillary column packed with porous and non-porous ODS stationary phases, high speed separation of 6 neutral aromatic compounds within 36 s by capillary electrochromatography (CEC) has been performed. Good reproducibility of the migration times for those solutes in high speed CEC was observed with RSD less than 1%. Both the linear velocity of EOF and the current linearly increases with the applied voltage, which means that the thermal effect by Joule heating was small. However, the capacity factor of solutes was found to decrease with the increase of the applied voltage, which was caused by the fact that about several seconds needed for the increase of voltage from 0 to applied value on a commercial CE instrument made larger contributions to the migration times of the early eluted compounds than those of lately eluted ones during high speed CEC, and voltage effect would increase with the higher applied voltage used. The linear relationship between the logarithm of capacity factor and the number of carbon for homologous compounds was observed, and positive value of slope means that the hydrophobicity of solutes is one of the main contribution factors to retention in high speed CEC packed with ODS stationary phases.

Large-pore mesoporous SBA-15 silica particles with submicrometer size as stationary phases for high-speed CEC separation

A new mesoporous sphere-like SBA-15 silica was synthesized and evaluated in terms of its suitability as stationary phases for CEC. The unique and attractive properties of the silica particle are its submicrometer particle size of 400 nm and highly ordered cylindrical mesopores with uniform pore size of 12 nm running along the same direction. The bare silica particles with submicrometer size have been successfully employed for the normal-phase electrochromatographic separation of polar compounds with high efficiency (e.g., 210 000 for thiourea), which is matched well with its submicrometer particle size. The Van Deemeter plot showed the hindrance to mass transfer because of the existence of pore structure. The lowest plate height of 2.0 mu m was obtained at the linear velocity of 1.1 mm/s. On the other hand, because of the relatively high linear velocity (e.g., 4.0 mm/s) can be generated, high-speed separation of neutral compounds, anilines, and basic pharmaceuticals in CEC with C-18-modified SBA-15 silica as stationary phases was achieved within 36, 60, and 34 s, respectively.

High-performance 1.55 mu m low-temperature-grown GaAs resonant-cavity-enhanced photodetector

A 1.55 mu m low-temperature-grown GaAs (LT-GaAs) photodetector with a resonant-cavityenhanced structure was designed and fabricated. A LT-GaAs layer grown at 200 degrees C was used as the absorption layer. Twenty- and fifteen-pair GaAs/AlAs-distributed Bragg reflectors were grown as the bottom and top mirrors. A responsivity of 7.1 mA/W with a full width at half maximum of 4 nm was obtained at 1.61 mu m. The dark current densities are 1.28x10(-7) A/cm(2) at the bias of 0 V and 3.5x10(-5) A/cm(2) at the reverse bias of 4.0 V. The transient response measurement showed that the photocarrier lifetime in LT-GaAs is 220 fs. (c) 2006 American Institute of Physics.

Characteristic analysis of the optical delay in frequency response of resonant cavity enhanced (RCE) photodetectors

With consideration of the modulation frequency of the input lightwave itself, we present a new model to calculate the quantum efficiency of RCE p-i-n photodetectors (PD) by superimposition of multiple reflected lightwaves. For the first time, the optical delay, another important factor limiting the electrical bandwidth of RCE p-i-n PD excluding the transit time of the carriers and RCd response of the photodetector, is analyzed and discussed in detail. The optical delay dominates the bandwidth of RCE p-i-n PD when its active layer is thinner than several 10 nm. These three limiting factors must be considered exactly for design of ultra-high-speed RCE p-i-n PD.

Fabrication and modulation characteristics of 1.3 mu m p-doped InAs quantum dot vertical cavity surface emitting lasers

We present the fabrication of 1.3 mu m waveband p-doped InAs quantum dot (QD) vertical cavity surface emitting lasers (VCSELs) with an extremely simple process. The continuous-wave saturated output power of 1.1 mW with a lasing wavelength of 1280 nm is obtained at room temperature. The high-speed modulation characteristics of p-doped QD VCSELs of two different oxide aperture sizes are investigated and compared. The maximum 3 dB modulation bandwidth of 2.5 GHz can be achieved at a bias current of 7 mA for a p-doped QD VCSEL with an oxide aperture size of 10 mu m in the small signal frequency response measurements. The crucial factors for the 3 dB bandwidth limitation are discussed according to the parameters' extraction from frequency response.

Silicon membrane resonant-cavity-enhanced photodetector

A Si resonant-cavity-enhanced (RCE) photodiode was fabricated on a silicon membrane. The Si membrane was formed by etching from the back side of the silicon-on-insulator substrate with the buried SiO2 layer as etch-stop layer. A gold layer was deposited serving as an electrode layer and bottom mirror of the RCE photodiode. The photodiode had an external quantum efficiency of 33.8% at the resonant wavelength of 848 nm and a full width at half maximum (FWHM) of 17 nm. The responsivity was 4.6 times that of a conventional Si p-i-n photodiode with the same absorption layer thickness. (c) 2005 American Institute of Physics.

Modulation response analysis of 1.3 mu m quantum dot vertical-cavity surface-emitting lasers

Some important parameters, such as gain, 3 dB bandwidth and threshold current of 1.3 mu m quantum dot vertical-cavity surface-emitting laser (QD VCSEL) are theoretically investigated. Some methods are developed to improve the VCSEL's modulation response. Significant improvement are prediced for p-type modulation doping. In connection with the threshold characteristic, we found that a structure with short cavity, multilayer quantum dots stack, p-type modulation doping and double intracavity contact on an un-doped DBR is much better suited to high speed quantum dot VCSELs. The parasitic effects of the VCSEL are,analyzed and the influence of packaging of the VCSEL on its modulation responds is analyzed.

Si1-xGex/Si resonant-cavity-enhanced photodetectors with a silicon-on-oxide reflector operating near 1.3 mu m

We report on a Si1-xGex/Si multiple quantum-well resonant-cavity-enhanced (RCE) photodetector with a silicon-on-oxide reflector as the bottom mirror operating near 1.3 mu m. The breakdown voltage of the photodetector is above 18 V and the dark current density at 5 V reverse bias is 12 pA/mu m(2). The RCE photodetector shows enhanced responsivity with a clear peak at 1.285 mu m and the peak responsivity is measured around 10.2 mA/W at a reverse bias of 5 V. The external quantum efficiency at 1.3 mu m is measured to be 3.5% under reverse bias of 16 V, which is enhanced three- to fourfold compared with that of a conventional p-i-n photodetector with a Ge content of 0.5 reported in 1995 by Huang [Appl. Phys. Lett. 67, 566 (1995)]. (C) 2000 American Institute of Physics. [S0003-6951(00)00628-8].

SHicon-based resonant-cavity-enhanced photodetectors

Silicon-based resonant-cavity-enhanced photodetectors (RCE-PD) with Si, Ge islands and InGaAs as absorption materials were introduced, respectively. The Ge islands and Si RCE-PD had a membrane structure and the Si-based InGaAs RCE-PDs were fabricated by bonding technology.

1.3 mu m GaInNAs/GaAs multiple-quantum-wells resonant-cavity-enhanced photodetectors

A GaInNAs/GaAs multiple quantum well (MQW) resonant-cavity enhanced (RCE) photodetector operating at 1.3 mum with the full-width at half-maximum of 5.5 nm was demonstrated. The GaInNAs RCE photodetector was grown by molecular-beam epitaxy using an ion-removed dc-plasma cell as nitrogen source. GaInNAs/GaAs MQW shows a strong exciton peak at room temperature that is very beneficial for applications in long-wavelength absorption devices. For a 100-mum diameter RCE photodetector, the dark current is 20 and 32 pA at biases of 0 and 6 V, respectively, and the breakdown voltage is -18 V. The measured 3-dB bandwidth is 308 MHz. The reasons resulting in the poor high speed property were analyzed. The tunable wavelength of 18 nm with the angle of incident light was observed.

Preparation of low-molecular-weight and high-sulfate-content chitosans under microwave radiation and their potential antioxidant activity in vitro

In the present paper microwave radiation has been used to introduce N-sulfo and O-sulfo groups into chitosan with a thigh degree of substitution and low-molecular weight. The sulfation of chitosan was performed in microwave ovens. It was found that microwave heating is a convenient way to obtain a wide range of products of different degrees of substitution and molecular weight only by changing reaction time or/and radiation power. Moreover, microwave radiation accelerated the degradation of sulfated chitosan, and the molecular weight of sulfated chitosan was considerably lower than that obtained by traditional heating. There are no differences in the chemical structure of sulfated chitosan obtained by microwave and by conventional technology. FTIR and C-13 NMR spectral analyses demonstrated that a significantly shorter time is required to obtain a satisfactory degree of substitution and molecular weight by microwave radiation than by conventional technology. In this present paper, we also determined antioxidant activity of low-molecular-weight and high-sulfate-content chitosans (LCTS). The results showed LCTS could scavenge superoxide and hydroxyl radical. Its IC50 is 0.025 and 1.32mg/mL, respectively. It is a potential antioxidant in vitro. (C) 2004 Published by Elsevier Ltd.

Underwater Acoustics and Cavitating Flow of Water Entry

The fluid mechanics of water entry is studied through investigating the underwater acoustics and the supercavitation. Underwater acoustic signals in water entry are extensively measured at about 30 different positions by using a PVDF needle hydrophone. From the measurements we obtain (1) the primary shock wave caused by the impact of the blunt body on free surface; (2) the vapor pressure inside the cavity; (3) the secondary shock wave caused by pulling away of the cavity from free surface; and so on. The supercavitation induced by the blunt body is observed by using a digital high-speed video camera as well as the single shot photography. The periodic and 3 dimensional motion of the supercavitation is revealed. The experiment is carried out at room temperature.