• Title/Summary/Keyword: chromatogram

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Glycomacropeptide Hydrolysed from Bovine K-Casein ; II. Chromatographic Changes of k-Casein Macropetide as Related to Trichloroacetic Acid Concentration (우유의 k-Casein에서 분해된 Glycomacropeptide에 관한 연구; II. Trichloroacetic Acid의 농도에 따른 k-Casein Macropeptide 분별 특성의 변화)

  • Moon Yong-Il;Lee Wonjae;Oh Sejong
    • Food Science of Animal Resources
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    • v.25 no.4
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    • pp.478-482
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    • 2005
  • Bovine k-casein macropeptide was prepared by adding TCA (3, 6, and $12\%$) treatment after chymosin reaction. Each TCA soluble macropeptide was fractionated into five peak by ion exchange column chromatography. In proportiion to TCA concentrations, the ratio of peak area showed different the elution pattern. At the 6 and $12\%$ TCA concentration, area ratio of P-I which did not content carbohydrates was decreased to 19.9 and $17.0\%$ of total peak area respectively. The area of P-III was changed from $10.2\%\;to\;26.2\;and\;13.2\%$ when the TCA concentration was increased from 3 to 6 and $12\%$ Cholera toxin binding activity of k-casein macropeptide eluted at $0.17\~0.18M$ NaCl gradient was not inhibited by 6 and $12\%$ TCA treatments. The use of $6\%$ TCA as extraction buffer was feasible and led to an effective separation of the peak III.

A Study of Morphology and Pattern Analysis in Magnoliae Cortex (후박(厚朴)의 외.내부형태 및 이화학패턴연구)

  • Lee, Guem-San;Kim, Jung-Hoon;Choi, Go-Ya;Kang, Dae-Hoon;Hwang, Sung-Yeoun;Jeong, Seung-Il;Kim, Hong-Jun;Ju, Young-Sung
    • The Korea Journal of Herbology
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    • v.23 no.4
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    • pp.21-29
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    • 2008
  • Objectives: To determine the standards for discrimination of Magnoliae Cortex, the experiment of specific external-internal characters and the physicochemical pattern analysis were performed. Methods: External characteristics was observed using a stereoscope. Paraffin-mediated sectioned materials were stained by Ju's method. Physicochemical patterns of materials were analyzed using HPLC. Results: 1. Botanical characteristics: Magnolia officinalis had one seed and a white flower, while M. obovata had two seeds and a white flower. Machilus thunbergii had berry and spherical fruits and yellowish green panicles. 2. External characteristics: M. officinalis and M obovata were dark and thick. M. officinalis was gray brown and greasy while M. obovata was light-gray, less oily and smoothly sectioned. Machilus thunbergii was thin and relatively light or yellow-brown, coarsely sectioned and faintly specific scents. 3. Internal characteristics: The bast parts of M. officinalis and M. obovata were commonly wider than Machilus thunbergii The cork cortex of M. officinalis was $10{\sim}mg/L$ cell layers with many oil cells, while that of M. obovata was $4{\sim}7$ cell layers with less oil cells. Machilus thunbergii's xylem which consisted of ring-shaped cambium at 1st and 2nd part was occupied in large portion. 4. Physicochemical pattern: Both M. officinalis and M. obovata involved honokiol and magnolol. All kinds of M. officinalis involved Magnatriol B but one kind of M. ovobata and all of Machilus thunbergii didn't. Machilus thunbergii showed different pattern of chromatogram from that of 2 species above. Conclusions: These results could be used as standards for discrimination of Magnoliae Cortex and as the method of objectification in medicinal herbs giving the basic resource for bioactivity research.

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Quantitation of Phthalate and Adipate in Natural Mineral Water and PET Container (먹는 샘물 및 PET 용기 중 Phthalate와 Adipate의 정량분석)

  • Shin, Ueon-Sang;Ahn, Hye-Sil;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.475-481
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    • 2002
  • The determination of phthalates and adipate in natural mineral water and its container is described. Phthalates and adipate were extracted from natural mineral water by liquid-liquid extraction with methylene chloride, concentrated and then injected in GC-MS (SIM). Phthalates and adipate from 1) PET, cap, label and glue were extracted in Soxhlet with 50 mL of carbon tetrachloride, purified with silicagel and detected with GC-MS (SIM). Peak shapes and quantitation of phthalates and adipate were excellent, with linear calibration curves over a range of $0.1{\sim}10{\mu}g/L$ in water sample ($r^2$ > 0.996) and over a range of $1{\sim}1,000{\mu}g/Kg$ in solid samples ($r^2$>0.994). The detection limits of analytes were $0.002{\sim}0.010{\mu}g/L$ in water and $0.01{\sim}0.02{\mu}g/Kg$ in solid samples. Five kinds of natural mineral water samples, two PETs, two labels, two caps and two glues were quantified by the described procedure. As a results, the concentrations of total phthalates in natural mineral water ranged from ND ~ 1.2 ng/mL. Otherwise, the concentrations of total phthalate extracted from PET ranged from 0.55 ~ 1.2 mg/Kg. We found that the accurate determination of phthalte and adipate in natural mineral water and container must be considered blank correction and the removal of label and glue in PET sample.

Pretreatment method of urinary thiodiglycolic acid as metabolite of vinyl chloride (염화비닐의 요중 대사물질인 thiodiglycolic acid의 분석을 위한 전처리 조건)

  • Hong, Joo Youn;Kim, Chi Nyon;Jung, Jae Hoon;Chang, Jung Hwan;Roh, Jaehoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.9 no.1
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    • pp.23-40
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    • 1999
  • The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

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Geographical origin discrimination of Korean variety, Angelica gigas Nakai by using TDU (Thermal Desorption Unit)-GC/MS (TDU-GC/MS를 이용한 한국품종 참당귀 국산 판별 기법)

  • Lee, Mi-Na;Kim, Yoon-Suk;Kim, Won-Il;Kim, Jeong-Gyu;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.63 no.1
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    • pp.29-33
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    • 2020
  • The objective of this study was to develop a fast and accurate method of variety discrimination and geographical discrimination origin of Korean angelica (Korean variety, Angelica gigas Nakai) by using TDU-GC/MS. Two peaks of decursin and decursinol, which are coumarin derivatives were identified in the range of Total Ion Chromatogram (TIC) RT 26.9-27.2 of the Korean angelica by GC/MS analysis at the time of condensation in a refrigerated condensation system after thermal desorption of sample extracts. In case of Chinese angelica (Chinese variety), ligustilide peak was detected at the RT 17.2. In order to investigate the difference of volatile components according to the geographical origin of Korean variety, the mass spectra were measured by TDU-GC/MS at the range of m/z 40-400 amu. The TIC of domestic cultivation and Chinese cultivation of the Korean variety, Angelica gigas Nakai showed the same tendency as a whole. However, in partial scans of TIC, two peaks detected at 15.54 and 16.05 of RT showed different peak patterns between Korean angelica (Korean variety) cultivated in Korea and in China. The ratio of Peak A (RT 15.54) and B (RT 16.05) was 0.0-0.2 for domestic cultivation and 0.5-2.8 for Chinese cultivation, confirming the possibility of discriminating origin by comparing the TIC peak pattern of TDU-GC/MS.

Quali-Quantitative Analysis of Flavonoids for Mulberry Leaf and Fruit of 'Suhyang'

  • Ju, Wan-Taek;Kwon, O-Chul;Lee, Min-Ki;Kim, Hyun-Bok;Sung, Gyoo-Byung;Kim, Yong-Soon
    • Korean Journal of Environmental Agriculture
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    • v.36 no.4
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    • pp.249-255
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    • 2017
  • BACKGROUND: Globally, mulberry (Morus sp.) is exploited for feeding leaf to silkworms in order to obtain silk fiber or for animal feedstock production. Also, mulberry fruit is known to a by-product that was produced from mulberry tree after harvesting leaves for silkworm rearing, as a yield and consumption of mulberry fruit was increased, it has been fixing to a newincome crop. Mulberry leaves and fruits are used for the health benefits of human beings. Mulberry contains various bioactive components, such as alkaloids and flavonoids. Mulberry flavonoids are an important part of the diet because of their effects on human nutrition. The flavonoids in mulberry leaf and fruit of 'Suhyang'(Morus alba L.) were determined. METHODS AND RESULTS: Flavonoids for mulberry leaf and fruit of 'Suhyang' were analysed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS)technique. An UPLC-DAD-QTOF/MS system was used, and identification of mulberry leaves constituents was carried out on the basis of the complementary information obtained from LC spectra, MS ions, and MS/MS fragments. The mulberry leaf (16 flavonoids) and fruit (9 flavonoids) were isolated and analyzed from Suhyang using UPLC-DAD-QTOF/MS chromatogram. To the best of our knowledge, Quercetin 3-O-(6"-O-malonyl) glucoside and quercetin 3-O-rutinoside (rutin) was detected on the highest content in leaf and fruit, respectively and further research will be devoted to evaluate their biological activity. CONCLUSION: Obtaining information about the concentration of functional materials in mulberry leaves could contribute to the development and promotion of processed, functional products and offer possible industrial use of 'Suhyang', holding promises to enhance the overall profitability of sericulture.

Expression of Paenibacillus macerans Cycloinulooligosaccharide Fructanotransferase in Saccharomyces cerevisiae (Saccharomyces cerevisiae에서 Paenibacilius macerans 유래 cycloinulooligosaccha-ride fructanotransferase의 발현)

  • Kim Hyun-Chul;Kim Jeong-Hyun;Jeon Sung-Jong;Choi Woo-Bong;Nam Soo-Wan
    • Journal of Life Science
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    • v.15 no.3 s.70
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    • pp.317-322
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    • 2005
  • The cycloinulooligosaccharide fructanotransferase (CFTase) gene (cft) from Paenibacillus macerans was subcloned into an E. coli-yeast shuttle vector, pYES2.0, resulting in pYGECFTN. The plasmid pYGECFTN (8.6 kb) was introduced into Saccharomyces cerevisiae SEY2102 cells and then the transformants were selected on the synthetic defined media lacking uracil. The cft gene expression in yeast transformant was demonstrated by the analyses cyclofructan (CF) spots on thin-layer chromatogram. The recombinant CFTase was not secreted into the medium and localized in the periplasmic space. The production of CF was observed after 5 min of the enzymatic reaction with inulin. The optimun pH and temperature for CF production were found to be at pH 8.0 and $45^{\circ}C$, respectively. Enzyme activity was stably maintained up to $55^{\circ}C$. The CF was produced from all inulin sources and was most efficiently produced from dahlia tubers and Jerusalem artichokes.

Free Sugar, Free Amino Acid, Non-Volatile Organic Acid and Volatile Compounds of Dongchimi added with Jasoja(Perillae semen) (자소자 첨가 동치미의 유리당, 유리아미노산, 비휘발성 유기산 및 휘발성 향기성분)

  • 황재희;장명숙
    • Korean journal of food and cookery science
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    • v.19 no.1
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    • pp.1-10
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    • 2003
  • All optional ingredient, Jasoja(Perillae semen) was adopted to improve Dongchimi in qualify during fermentation. Free sugar, free amino acid, non-volatile organic acid and volatile compounds were determined during fermentation at 10$^{\circ}C$ for 45 days. Free sugar content was slightly higher in 0.5%-Jasoja-treated samples than that of control. The contents of free amino acids in control Dongchimi (without jasoja) increased slowly during fermentation while those in 0.5 %-treated samples began to decrease after reaching their maximum value on the day 11 when Dongchimi became most acceptable. There were 6 non-volatile organic acids, such as lactic, fumaric, succinic, malic, tartaric, and citric acid. Among these, only lactic and succinic acid increased consistently with fermentation while others decreased. Volatile components in Dongchimi were mostly identified as sulfur-containing compounds by gas chromatography. Their numbers and % peak areas in the gas chromatogram decreased slightly with the increase in organic acids and alcohols during fermentation period. On the other hand, Dongchimi prepared with Jasoja maintained its contents of total acids as well as the level of sulfur-containing compounds.

Comparison of Different Solid-Phase Extraction Methods for the Analysis of Heterocyclic Amines from Pan-Fried Pork Meat (가열 조리된 돼지고기의 Heterocyclic Amines 분석을 위한 Solid-phase 추출 방법의 비교)

  • Lee, Jae-Hwan;Back, Yu-Mi;Lee, Kwang-Geun;Shin, Han-Seung
    • Food Science of Animal Resources
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    • v.28 no.5
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    • pp.637-644
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    • 2008
  • Four different extraction and purification methods were evaluated to determine the heterocyclic amines (HCAs) in fried pork patties. Pork patties were cooked in the teflon-coated electric frying pan at $230^{\circ}C$ for 8 min per side. HCAs in the fried pork patties were extracted and purified using four different solid-phase extraction (SPE) methods and quantitated by LC-MS (API-ESI). Recovery of four different extraction and purification methods was evaluated by comparing the HCAs amounts quantified by the standard addition method. Validation of extraction and purification methods for fried pork patties was determined to establish accurate sample preparation. The recoveries of HCAs from different SPE methods were calculated. The recovery yields were 15.7-68.7% (Polar amine group) and 25.0-74.7% (less-polar amine group) in method A. Method D provided recovery yields ranging from 14.1% to 68.7% in polar amine groups and from 3.0% to 72.3% in less-polar amine groups, respectively. Modified procedures of Method A and D were the most suitable extraction and purification method for HCAs analysis from fried pork patties.

Separation of Highly Purified Antimicrobial Lysozyme Using Ultrafiltration and Characteristics of Membrane Fouling (한외여과 공정을 이용한 고순도 향균 Lysozyme 의 분리 및 막 침착 특성)

  • Lee, Eun-Young;Woo, Gun-Jo
    • Korean Journal of Food Science and Technology
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    • v.31 no.2
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    • pp.458-464
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    • 1999
  • The value of lysozyme as a natural food preservative is continuously increased due to its unique antimicrobial activity. To determine the optimum separation concentration among the various hen egg white protein (HEWP) concentrations (0.25, 0.5, 1.0, w/v), protein concentrations, lysozyme concentrations, specific activities (SA), and purification factors of prefiltered solution (PFS) and PM30 permeate solution (PMS) were compared. The purity of lysozyme separated at each step was analyzed and confirmed by gel permeation chromatography and electrophoresis. The fouling deposits on membrane were observed by SEM. The non-enzymatic proteins were removed over 99% by ultrafiltration (UF). The increased feed concentration did not contribute to the increase of SA. SA of PMS was 18 to 31 times higher than that of PFS. The optimum feed concentration was decided as 0.25% based on SA and purification factor. The non-enzymatic region of gel chromatogram was proved to be ovalbumin. The thickness of deposit on the UF membrane was approximately $0.9{\mu}m$ and removed by cleaning with 0.1 N NaOH. Therefore, UF using PM30 membrane was very effective to separate the antimicrobial lysozyme from various HEWPs.

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