• YAKHAK HOEJI
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• v.45 no.1
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• pp.34-38
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• 2001

The Phellodendri Cortex of Phellodendron amurense (Rutaceae) is known to contain a number of isoquinoline alkaloid, and berberine, palmatine, jateorrhizine, phellodendrine and magnoflorine are the major constituents of protoberberine alkaloids. For the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation, the new spectrophotometric method was developed with a simple and selective sample clean-up using thiocyanatocobaltate[II] complex ion. Samples were extracted with 0.1 mM hydrochloric acid, potassium biphthalate reagent, thiocyanatocobaltate reagent and 1.2-dichloroethane for 60 min. The absorbance of protoberberine alkaloid complexes in 1.2-dichloroethane solution was measured at 625 nm. Calibration curve for berberine was linear over the concentration range of 0.05~0.30 mg/ml 1.2-dichloroethane. The method proved to be rapid, simple and reliable for the determination of protoberberine alkaloids from Phellodendri Cortex and berberine chloride from the preparation.

• Macromolecular Research
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• v.16 no.2
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• pp.108-112
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• 2008

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) analysis of nonpolar polymeric materials is affected by the sample preparation as well as the matrix and cationizing agent. This study examined the influence of silver salt types on the MALDI analysis of polybutadiene (PB). Silver trifluoroacetate (AgTFA), silver benzoate (AgBz), silver nitrate ($AgNO_3$), and silver p-toluenesulfonate (AgTS) were used as the silver salts to compare the MALDI mass spectra of PB. The mixture solution of PB and 2,5-dihydroxybenzoic acid (DHB), as a matrix dissolved in THF, was spotted on the sample plate and dried. A droplet of the aqueous silver salt solution was placed onto the mixture. The mass spectrum with AgBz showed the clear $[M+Ag]^+$ ion distribution of PB while the mass spectrum with AgTFA did not show $[M+Ag]^+$ ions but only silver cluster ions. The mass spectra with $AgNO_3$ and AgTS did not show a clear $[M+Ag]^+$ ion distribution. The difference in the formation of $[M+Ag]^+$ ions of PB depending on the silver salts was attributed to the silver cation transfer reaction between the silver salt and the matrix (DHB). The mass spectrum showed a clear $[M+Ag]^+$ ion distribution of PB when the conjugate acid of the silver salt was less acidic than the matrix.

• Journal of the Korean Society of Food Science and Nutrition
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• v.24 no.6
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• pp.990-997
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• 1995

Effect of preparation method on Yulmoo kimchi(watery kimchi prepared with Yulmoo, leaf radish) fermentation was investigated by measuring physicochemical, microbiological and sensory properties for 20 days. Yulmoo kimchi was fermented at 4$^{\circ}C$ after keeping at room temperature(27$\pm$0.5$^{\circ}C$) for 8 hours. Four types(A, B, C, D) of Yulmoo kimchi were prepared. Sample A was made without wheat flour paste and red pepper powder and sample B was made with wheat flour paste. Sample C was made with red pepper powder, and sample D was made with wheat flour paste and red pepper powder. pH was slowly lowered and stabled after 10 days in all samples. Total acid content increased in all samples. Reducing sugar content initially increased and decreased thereafter. Especially, reducing sugar content of sample B increased in the early stage of fermentation and maintained initial reducing sugar content after 20 days. Total vitamin C content reduced during fermentation in all samples. Especially initial total vitamin C content of sample D increased more than those of other samples relatiely. Lightness and yellowness showed no difference, but on the other hand redness increased gradually in all samples. The number of lactic acid bactgeria reached maximum value in 10~13 days with the total cell numbers and gradually decreased thereafter in all samples. The number of lactic acid bacteria and total cell number of sample D was much more than those of any other samples. As a result of the sensory evaluation, Yulmoo kimchi showed significant difference in all characteristics. Sample D showed the highest scores in all characteristics before 10 days of fermentation. However, after 10 days sample B showed the highest scores.

• Geomechanics and Engineering
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• v.14 no.2
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• pp.131-139
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• 2018

The preparation of repeatable and uniformly reconstituted soil specimens up to the specified conditions is an essential requirement for the laboratory tests. In this study for large samples replication, the simultaneous usage of the traveling pluviation and curtain raining technique is used to develop a new method, called the curtain travelling pluviator (CTP). This simple and cost effective system is based on the air pluviation approach, whilst reducing the sample production time, can reproduce uniform samples with relative densities ranging from 25% to 96%. In order to investigate the resulting suitability and uniformity from the proposed method, a series of tests is performed. The effect of curtain traveling velocity, curtain width, drop height, and flow rate on the parameters of the sample is thoroughly investigated. Increase in the curtain velocity and drop height leads to the increase in relative density for the sand specimen. Increase in curtain width typically resulted in the reduction of relative density. Test results reveal that the terminal drop height for the sand specimen in this study is more than 500 mm. Relative density contour lines are presented that can be utilized in optimizing the drop height and curtain width parameters. Sample uniformity in the vertical and horizontal orientation is investigated through the sampling containers. Increasing relative density tends to result in the higher sample repeatability and uniformity.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.34 no.s01
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• pp.26-32
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• 1989

The analytic principles of GC and MS were explained in relation to plant hormone analyses and the characteristics of two instruments were compared. The selection of column, condition of measurement and the method of ionization to get a good spectrum were also briefly described. Finally, the pre-treatment of sample by solvent extraction method to remove the unnecessary part of sample and the synthetic method, especially reagents and reaction condition, for the preparation of ether or ester derivative which can be easily vaporized in GC were explained.

• Journal of the Korean Society of Tobacco Science
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• v.36 no.1
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• pp.26-33
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• 2014

Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

• Environmental Mutagens and Carcinogens
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• v.15 no.2
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• pp.106-114
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• 1995

A method was developed to detect total mutagenicity of fried fish for S. typhimurium TA98, using Ames assay. Method described herein circumvented problems associated with the sample preparation for Ames assay, i.e., a multi-purification step of sample and interference with solvent residuals. Experiment A, the best method developed in the present study, consisted of two important steps: pH adjustment of the aqueous sample solution from fried fish samples to remove impurities, and simultaneous distillation extraction (SDE) for partially purified samples to remove volatile compounds from solvents. The procedure and results were described as below. Fillet of gizzard shad (Konosirus punctatus) fish sample fried for 10 min each side on the temperature-controlled fry-pan (210$\circ$C) was homogenized in an aqueous acidic solution (pH 2) with a homogenizer, followed by filtration through Celite. The tiltrate (pH 2), removed some impurities by extraction with chloroform:methanol (2:1, v/v) mixture, was adjusted pH to 10 and then centrifuged to remove precipitate. The ethylacetate extract from the tiltrate of pH 10 was rotoevaporated and purified by SDE apparatus for 2 hours. Experiment A revealed significantly higher revertants (1928 per 25 g fried sample) than other Experiment (B, C, or D) tested. Experiment A gave good results in the mutagenicity test of fried fish sample with few purification steps using only 25 g fried sample and 650 ml of solvents; and thus this method could be a useful tool for the screening the mutagenicity or antimutagenicity of other foods as well.

• Journal of the Korean Society of Tobacco Science
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• v.32 no.2
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• pp.70-76
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• 2010

A simple and sensitive automatic amino acid analyzer method for the determination of free amino acids in tobacco was described. Sample preparation consisted of a single step of extraction with 0.1 mol HCl at ambient temperature in 60 min by sonication, followed by filtration of an aliquot. Automated amino acid analyzer was used to construct a post-column ninhydrin reaction unit to monitor amino acids separated by liquid chromatography using a series of eluting buffers. By optimization of sample preparation, separation of 19 amino acids was achieved. Limits of quantitation was 0.01 mg/g, coefficients of variation ranged from 0.5 % to 8.9 % and recoveries range from 85 % to 106 %. The method was applied to the analysis of amino acids contents of tobacco leaves in different varieties.

• Biomedical Science Letters
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• v.13 no.4
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• pp.361-368
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• 2007

Biological samples can be fixed either by chemical method by using chemical solution or physical methods by using heat treatment. The problem in traditional heat fixation is unsatisfactory quality due to uneven heat conduction in specimen and loss of inner cell contents. Chemical fixation method also bears several intrinsic problems like the limit in specimen size, time consumption in fixative impregnation, and loss of low molecular weight cell components. These factors deteriorate the quality of fixed specimen, thus limit the magnification and contrast of tissue pictures. Microwave heat has been reported to be a good alternative to current chemical methods to overcome these problem. In this study, we tried to introduce the microwave energy method to routine fixation work in hospital. We replaced chemical fixative with saline to provide moderate reaction condition, and used frozen section to reduce time for sample preparation. Temperature was measured at each experiment. The fixation of rat kidney tissue with 2.45 GHz electromagnetic wave and saline showed similar result to the control group fixed with traditional chemical method. Human tumor tissue fixed with 2.45 GHz electromagnetic in frozen section was improved in terms of histochemistry of PAS and immunohistochemistry of tumor marker like cytokeratin. Total turnaround time was reduced from $24\sim38$ h to to $2\sim4$ h. In conclusion, the quality of samples prepared by microwave heating method was at least as good as that of traditional method. If the condition for the fixation of different specimens is standardized, this new method could be applied to routine work in hospital, and could save working time as well.

• YAKHAK HOEJI
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• v.33 no.4
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• pp.241-245
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• 1989

A new application of high performance liquid chromatography for the determination of capsaicin and dihydrocapsaicin in cataplasma preparation was investigated. Optimum conditions for a good separation and detection were determined; 0.93 volt, acetonitrile: $H_3PO_4$ sol (pH 2.8), sample size; $7\;{\mu}l$. Recovery rates of capsaicin and dihydrocapsaicin from mixed artificial preparations were 99.9% and 98.4% respectively. Also reproducibility tests showed that the coefficient of variation was 1.59% for capsaicin and 1.14% for dihydrocapsaicin. There was no interference with cataplasma preparation containing thymol, dl-camphor and the commonly encountered excipients or additives such as gelatine, glycerine. This method was rapid, accurate and it gave higher sensitivity than other method.