Longhu Wang

GC-MS of volatile components of Schisandra chinensis obtained by supercritical fluid and conventional extraction.

In this paper, the volatile compounds of Schisandra chinensis obtained by different extraction techniques including supercritical fluid extraction (SFE), steam distillation (SD), Soxhlet extraction (SE) and ultrasound-assisted extraction (UAE) were investigated for the first time. The sample preparation procedure for GC-MS analysis of the volatile compounds was optimized and then 37, 45, 27 and 37 compounds were identified in the samples obtained by SFE, SD, SE and UAE methods, respectively. As the therapeutic effect of the traditional Chinese medicine is usually based on multifarious essential components or the combination of them instead of only one component, the volatile compounds were compared in groups with the extracts by SE, SD and UAE. This would be more reasonable to evaluate the effects of an alternative technique to extracting multifarious essential components. Among the identified components in the SFE extract, 32 compounds were the same as that by three conventional methods, accounting for 90.5% of the volatile compounds identified. However, as the volatile compounds were classed into groups, it was easy to see that the Schisandra chinensis oil extracted by SFE was made up largely of aromatics and sesquiterpenoids (52.1 and 27.6%, respectively), with less amounts of monoterpenoids and other compounds, distinguishing SFE from the conventional extractions.

Orthogonal array design for the optimization of supercritical fluid extraction of tanshinones from Danshen.

Different from the west medicine, the therapeutic effect of the traditional Chinese medicine is usually based on multifarious essential components or the combination of them instead of only one component. In this paper, a novel supercritical fluid extraction (SFE) method has been developed for extracting tanshinones (dihydrotanshinone I, cryptotanshinone, tanshinone I, and tanshinone II(A)) from Danshen, the dried root of Salvia miltiorrhiza. Various experimental conditions were investigated to optimize the SFE. Under the appropriate conditions, extracting at 40 MPa, and 50 degrees C and with CO(2) flow rate of 25 L/h for 1 h, SFE can achieve a better yield as well as the recoveries of the tanshinones than the conventional extraction using methanol. Moreover, the target compounds were analyzed by HPLC with a C(18) RP column by gradient elution using ACN and water as mobile phase at a flow rate of 1.0 mL/min and with UV detection at 270 nm. Four calibration equations were then established and good linear relationships were shown (r(2) >0.999) in the investigated concentration range. The recoveries, measured at three concentration levels, varied from 97.2 to 103.8%. The method provided in this article could be applied as an improved quality control method for Danshen products.

Monitoring of Antisolvent Crystallization of Sodium Scutellarein by Combined FBRM–PVM–NIR

Antisolvent crystallization can be used as an alternative to cooling or evaporation for the separation and purification of solid product in the pharmaceutical industry. To improve the process understanding of antisolvent crystallization, the use of in-line tools is vital. In this study, the process analytical technology (PAT) tools including focused beam reflectance measurement (FBRM), particle video microscope (PVM), and near-infrared spectroscopy (NIRS) were utilized to monitor antisolvent crystallization of sodium scutellarein. FBRM was used to monitor chord count and chord length distribution of sodium scutellarein particles in the crystallizer, and PVM, as an in-line video camera, provided pictures imaging particle shape and dimension. In addition, a quantitative model of PLS was established by in-line NIRS to detect the concentration of sodium scutellarein in the solvent and good calibration statistics were obtained (r(2) = 0.976) with the residual predictive deviation value of 11.3. The discussion over sensitivities, strengths, and weaknesses of the PAT tools may be helpful in selection of suitable PAT techniques. These in-line techniques eliminate the need for sample preparation and offer a time-saving approach to understand and monitor antisolvent crystallization process.

Influences of sub-Alfvenic shear flows on nonlinear evolution of magnetic reconnection in compressible plasmas

Influences of sub-Alfvenic shear flows on the nonlinear evolution of the magnetic reconnection are studied in the framework of compressible resistive MHD and compressible Hall MHD. It is found for the first time that the sub-Alfvenic shear flow can either stabilize or destabilize magnetic reconnection, which is mainly determined by the plasma beta and the half thickness of the shear flow ( λ v ). The shear flow exhibits a suppressing effect on magnetic reconnection and the boosting effect nearly disappears for the beta plasma β ≲ 1 , which is associated with the presence of a pair of discontinuities in the upper and lower inflow region. The shear flow has the boosting effect on magnetic reconnection when the half thickness of the shear flow exceeds a critical value in the high beta plasma which is in a good agreement with the results from incompressible simulation. With the inclusion of the Hall effect,shear flow can still either stabilize or destabilize magnetic reconnection, but the boosting effect becomes weaker as the ion inertial length d i increases.

Monte Carlo study of critical scaling and universality in non-equilibrium short-time dynamics

Abstract We investigated the critical scaling and universality of the short-time dynamics for the spin models on the two-dimensional triangle lattices. By using the Monte Carlo simulations, the short-time dynamic scaling is verified, and the critical exponents θ , z and β / ν are estimated from the power-law behavior of the magnetization, auto-correlation and second magnetic moment. Our results confirmed the universality proposal.

Fast Quantification of Phenylethyl Alcohol in Rose Water and Chemical Profiles of Rose Water and Oil of Rosa damascena and Rosa rugosa from Southeast China

A new and effective high performance liquid chromatography (HPLC) method was developed for fast quantification of phenylethyl alcohol in rose water. Chemical profiles of rose water and oil of Rosa damascena and Rosa rugosa from Southeast China were investigated by gas chromatography (GC) and gas chromatography–mass spectrometry (GC–MS). Fast HPLC was achieved by rapid sample preparation and fast elution using acetonitrile–water (35:65, v/v) on Zorbax SB-C18. It was validated and applied to rapid analysis of different rose water samples, in which the contents of phenylethyl alcohol ranged from 454.6 to 526.7 µg/mL. GC and GC–MS revealed that rose water volatiles of R. damascena and R. rugosa mainly consisted of phenylethyl alcohol (90.2% and 78.7%, respectively) and citronellol (4.5% and 13.5%, respectively). This is the first report on fast HPLC quantification of phenylethyl alcohol in rose water and chemical profiles of rose water volatiles of R. damascena and R. rugosa from Southeast China. The developed HPLC method can serve as a fast quality control during rose water production.

Development and validation of a HPLC method for the determination of five bioactive compounds in the "Xuebijing" injection.

A reversed phase high performance liquid chromatographic (RP-HPLC) method with ultraviolet (UV) detector was developed for simultaneously determining five bioactive components (i.e., hydroxysafflor yellow A: HSYA; paeoniflorin, ferulic acid, benzoic acid, and danshensu) in “Xuebijing” (XBJ) injection, a widely used traditional Chinese medicine (TCM) for treating sepsis and multiple organ dysfunction syndrome. A Zorbox SB C18 column was used with 0.2% phosphoric acid (V/V)-acetonitrile as the mobile phase under the condition of gradient elution. The five components were analyzed by using a timed wavelength measure according to their maximum absorption wavelength. The intraday and interday precisions of the five investigated compounds were less than 1.17% and the average recoveries ranged from 97.3% to 103.2%. There were good linear correlations between the concentrations of the five components and their chromatographic peak areas (R2 ≥ 0.9998), the proposed method was successfully applied to determine the five components in different batches of XBJ injection products, the results indicated that the proposed method is simple, stable, and accurate and could be readily utilized as a quality control method for manufacturing process of XBJ injection.

A novel HPLC method to analyze imperatorin and isoimperatorin of Angelica dahurica oils obtained by supercritical fluid extraction.

Abstract In this paper, a novel HPLC method was developed for analyzing imperatorin and isoimperatorin in the SFE extracts of Angelica dahurica. The separations were effected by using a mobile phase of methanol and water. The gradient elution of the mobile phase was 80% in 0–5 min, 80–68% in 5–7 min, and 68% in 7–12 min. The detector wavelength was set at 249 nm. Analytical characteristics of the separation, such as limit of detection, limit of quantification, linear range, and reproducibility were evaluated. The developed method was applied to optimizing supercritical fluid extraction of coumarins from Angelica dahurica. The maximum extraction yield was obtained at 30 MPa and 50°C with a flow rate of 25 L/h and extraction time of 2 h.

Water-soluble essential oil components of fresh flowers of Osmanthus fragrans Lour

Abstract Water-soluble essential oil components of Osmanthus fragrans fresh flowers were recovered from the hydrolate and the cold infusion, byproducts of essential oil isolation and concrete extraction, respectively. Chemical investigation was performed by gas chromatography (GC) and gas chromatography – mass spectrometry (GC-MS). As a comparative study, the Clevenger-distilled, decanted and absolute oils were also analyzed. The oil recovered from the hydrolate was mainly composed of cis-linalool oxide (furanoid) (51.4%) and trans-linalool oxide (furanoid) (37.8%). This oil presented 0.024 ± 0.004% (w/w) relative to the fresh flowers, and accounted for 25.5 ± 5.8% of the total oil (decanted + recovered). The oil recovered from the cold infusion was rich in 4-methoxyphenethyl alcohol (31.0%), 4-hydroxyphenethyl alcohol (18.0%), cis-linalool oxide (furanoid) (9.8%), cis-linalool oxide (pyranoid) (8.9%) and trans-linalool oxide (furanoid) (7.3%). This oil accounted for 0.018 ± 0.003% (w/w) of the fresh flowers. In summary, the recovered water-soluble oils are valued for being rich in compounds characteristic of O. fragrans and can find applications in the essential oil industry.

Pilot-Scale Multi-Stage Countercurrent Extraction of Scutellarein from Erigeron breviscapus (Vant.) Hand-Mazz

Abstract A low-temperature, timesaving, lower solvent consumption, and energy cost and multi-stage countercurrent extraction (MCCE) technique was developed for pilot-scale production of scutellarein from Erigeron breviscapus (Vant.) Hand-Mazz. The optimum conditions of MCCE process were obtained using the orthogonal array design method, i.e., 70% (v/v) of ethanol water solution, 16 L/kg of solvent to herbal sample ratio, 45°C of extraction temperature and 30 min of extraction time. A comparison between the MCCE technique and single pot extraction (SPE) under respective optimized operation conditions was made and time courses of scutellarein of MCCE and SPE processes were plotted, indicating that the MCCE technique can lower the extraction temperature and decrease five-sixth of the extraction time and two-thirds of the solvent consumption at the equivalent extraction yield of scutellarein.