Extraction of Nitraria tangutorum seed oil by supercritical carbon dioxide and determination of free fatty acids by HPLC/APC/IMS with fluorescence detection

The seed oil from Nitraria tangutorum samples was obtained by supercritical carbon dioxide extraction methods. The extraction parameters for this methodology, including pressure, temperature, particle size and extraction time, were optimized. The free fatty acids in the seed oil were separated with a pre-column derivation method and 1,2-benzo-3,4-dihydrocarbazole-9-ethyl-p-toluenesulfonate (BDETS) as a labeling regent, followed by high-performance liquid chromatography (HPLC) with fluorescence detection. The target compounds were identified by mass spectrometry with atmospheric pressure chemical ionization (APCI in positive-ion mode). HPLC analysis shows that the main compositions of the seed oil samples were free fatty acids (FFAs) in high to low concentrations as follows: linoleic acid, oleic acid, hexadecanoic acid and octadecanoic acid. The assay detection limits (at signal-to-noise of 3:1) were 3.378-6.572 nmol/L. Excellent linear responses were observed, with correlation coefficients greater than 0.999. The facile BDETS derivatization coupled with mass spectrometry detection allowed the development of a highly sensitive method for analyzing free fatty acids in seed oil by supercritical CO2 extraction. The established method is highly efficient for seed oil extraction and extremely sensitive for fatty acid profile determination. (C) 2007 Elsevier B.V. All rights reserved.

Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS)

A sensitive method for the determination of 30 kinds of free fatty acids (FFAs, C-1-C-30) with 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4,5-f] 9,10-phenan- threne (TSPP) as labeling reagent and using high performance liquid chromatography with fluorescence detection and identification by online postcolumn mass spectrometry with atmospheric pressure chemical ionization (APCI) source in positive-ion mode (HPLC/MS/APCI) has been developed. TSPP could easily and quickly label FFAs in the presence of K2CO3 catalyst at 90 degrees C for 30 min in N,N-dimethylformamide (DMF) solvent, and maximal labeling yields close to 100% were observed with a 5-fold excess of molar reagent. Derivatives were stable enough to be efficiently analyzed by high performance liquid chromatography. TSPP was introduced into fatty acid molecules and effectively augmented MS ionization of fatty acid derivatives and led to regular MS and MS/MS information. The collision induced cleavage of protonated molecular ions formed specific fragment ions at m/z [MH](+)(molecular ion), m/z [M'+CH2CH2](+)(M' was molecular mass of the corresponding FFA) and m/z 295.0 (the, mass of protonated molecular core structure of TSPP). Fatty acid derivatives were separated on a reversed-phase Eclipse XDB-C-8 column (4.6 x 150 mm, 5 mu m, Agilent) with a good baseline resolution in combination with a gradient elution. Linear ranges of 30 FFAs are 2.441 x 10(-3) to 20 mu mol/L, detection limits are 3.24 similar to 36.97 fmol (injection volume 10 mu L, at a signal-to-noise ratio of 3, S/N 3:1). The mean interday precision ranged from 93.4 to 106.2% with the largest mean coefficients of variation (R.S.D.) < 7,5%. The mean intraday precision for all standards was < 6.4% of the expected concentration. Excellent linear responses were observed with correlation coefficients of > 0.9991. Good compositional data could be obtained from the analysis of extracted fatty acids from as little as 200 mg of bryophyte plant samples.Therefore, the facile TSPP derivatization coupled with HPLC/MS/APCI analysis allowed the development of a highly sensitive method for the quantitation of trace levels of short and long chain fatty acids from biological and natural environmental samples.

基于显式分形插值的高保真地震数据重建方法研究

Based on the fractal theories, contractive mapping principles as well as the fixed point theory, by means of affine transform, this dissertation develops a novel Explicit Fractal Interpolation Function（EFIF）which can be used to reconstruct the seismic data with high fidelity and precision. Spatial trace interpolation is one of the important issues in seismic data processing. Under the ideal circumstances, seismic data should be sampled with a uniform spatial coverage. However, practical constraints such as the complex surface conditions indicate that the sampling density may be sparse or for other reasons some traces may be lost. The wide spacing between receivers can result in sparse sampling along traverse lines, thus result in a spatial aliasing of short-wavelength features. Hence, the method of interpolation is of very importance. It not only needs to make the amplitude information obvious but the phase information, especially that of the point that the phase changes acutely. Many people put forward several interpolation methods, yet this dissertation focuses attention on a special class of fractal interpolation function, referred to as explicit fractal interpolation function to improve the accuracy of the interpolation reconstruction and to make the local information obvious. The traditional fractal interpolation method mainly based on the randomly Fractional Brown Motion (FBM) model, furthermore, the vertical scaling factor which plays a critical role in the implementation of fractal interpolation is assigned the same value during the whole interpolating process, so it can not make the local information obvious. In addition, the maximal defect of the traditional fractal interpolation method is that it cannot obtain the function values on each interpolating nodes, thereby it cannot analyze the node error quantitatively and cannot evaluate the feasibility of this method. Detailed discussions about the applications of fractal interpolation in seismology have not been given by the pioneers, let alone the interpolating processing of the single trace seismogram. On the basis of the previous work and fractal theory this dissertation discusses the fractal interpolation thoroughly and the stability of this special kind of interpolating function is discussed, at the same time the explicit presentation of the vertical scaling factor which controls the precision of the interpolation has been proposed. This novel method develops the traditional fractal interpolation method and converts the fractal interpolation with random algorithms into the interpolation with determined algorithms. The data structure of binary tree method has been applied during the process of interpolation, and it avoids the process of iteration that is inevitable in traditional fractal interpolation and improves the computation efficiency. To illustrate the validity of the novel method, this dissertation develops several theoretical models and synthesizes the common shot gathers and seismograms and reconstructs the traces that were erased from the initial section using the explicit fractal interpolation method. In order to compare the differences between the theoretical traces that were erased in the initial section and the resulting traces after reconstruction on waveform and amplitudes quantitatively, each missing traces are reconstructed and the residuals are analyzed. The numerical experiments demonstrate that the novel fractal interpolation method is not only applicable to reconstruct the seismograms with small offset but to the seismograms with large offset. The seismograms reconstructed by explicit fractal interpolation method resemble the original ones well. The waveform of the missing traces could be estimated very well and also the amplitudes of the interpolated traces are a good approximation of the original ones. The high precision and computational efficiency of the explicit fractal interpolation make it a useful tool to reconstruct the seismic data; it can not only make the local information obvious but preserve the overall characteristics of the object investigated. To illustrate the influence of the explicit fractal interpolation method to the accuracy of the imaging of the structure in the earth’s interior, this dissertation applies the method mentioned above to the reverse-time migration. The imaging sections obtained by using the fractal interpolated reflected data resemble the original ones very well. The numerical experiments demonstrate that even with the sparse sampling we can still obtain the high accurate imaging of the earth’s interior’s structure by means of the explicit fractal interpolation method. So we can obtain the imaging results of the earth’s interior with fine quality by using relatively small number of seismic stations. With the fractal interpolation method we will improve the efficiency and the accuracy of the reverse-time migration under economic conditions. To verify the application effect to real data of the method presented in this paper, we tested the method by using the real data provided by the Broadband Seismic Array Laboratory, IGGCAS. The results demonstrate that the accuracy of explicit fractal interpolation is still very high even with the real data with large epicenter and large offset. The amplitudes and the phase of the reconstructed station data resemble the original ones that were erased in the initial section very well. Altogether, the novel fractal interpolation function provides a new and useful tool to reconstruct the seismic data with high precision and efficiency, and presents an alternative to image the deep structure of the earth accurately.