• Title/Summary/Keyword: sample pretreatment

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Analysis of Chemical Warfare Agents in Water Using Single-Drop Microextraction

  • Park, Yang-Gi;Kim, Sung-Ki;Choi, Ki-Hwan;Son, Byung-Hoon;Park, Ju-Sub;Kang, Hong-Ku
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.49-52
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    • 2009
  • Single-drop microextraction (SDME) is an extraction methodology where the drop plays an essential role as extracts. It was evaluated for the GC-MS determination of nerve agents, one class of the chemical warfare agents (CWAs). Since these nerve agents are highly toxic, it is important to detect the nerve agents in the environmental samples. Several affecting factors including extraction solvents, stirring rate, extraction time, and amounts of salt were optimized. The limit of detections (LODs) were 0.1 - 10 ng/mL and the relative standard deviations (RSDs%, n=5) were in the range of 6.3% to 9.0% for four nerve agents. Without pretreatment of the environmental samples, 5-103 fold enrichments and 48-100% recovery were accomplished. These results demonstrated the feasibility of this method for on-site and off-site analysis of water sample collected from suspicious CWAs site.

Recent Development of Laboratory-made Solid-phase Microextraction Fibers on the Application of Food Safety Analysis

  • Zeng, Jingbin;Chen, Jinmei;Chen, Wenfeng;Huang, Xiaoli;Chen, Liangbi;Chen, Xi
    • Food Science and Biotechnology
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    • v.18 no.3
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    • pp.579-585
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    • 2009
  • Solid-phase microextraction (SPME) has gained widespread acceptance in sample pretreatment due to its solvent-free and easy-to-operate properties. SPME fibers are considered as a key part of SPME technique, since it primarily determines the extraction performance of the method including sensitivity, selectivity, and reproducibility. Generally speaking, target analyte with different chemical property requires fiber coating that has the best affinity towards it. Due to the lack of varieties of commercial fibers available currently, considerable efforts have been recently made to develop tailor-made fibers to fulfill increasing demands of different analysis. This paper concisely classify some SPME fiber preparation approaches such as sol-gel technology, physical deposition, molecularly imprinted technique, and their respective application in food safety analysis.

Determination of L-Carnitine in Infant Powdered Milk Samples after Derivatization

  • Park, Jung Min;Koh, Jong Ho;Kim, Jin Man
    • Food Science of Animal Resources
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    • v.41 no.4
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    • pp.731-738
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    • 2021
  • Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.

Evaluation of Effects on Tritium Measurement According to HTO Type Sample Preparation Conditions (HTO 형태 시료 조제 조건에 따른 삼중수소 계측에 미치는 영향 평가)

  • An, Eun-Mi;Kim, Jung-Hoon;Lee, Hong-Yeon;Han, Sang-Jun;Kim, Bo-Gil
    • Journal of radiological science and technology
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    • v.44 no.4
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    • pp.381-387
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    • 2021
  • In this study, for the measurement of 3H(tritium) radioactivity concentration, a study was conducted on whether the type of cocktail and the material of the vial had an effect on the measurement before liquid scintillation counter measurement on HTO-type samples that had undergone physical and chemical pretreatment. As a result of the study, the efficiency according to the type of cocktail was higher in Ultima Gold LLT than Ultima Flo-AP cocktail with polyethylene (1.49%), glass (5.10%), and teflon (6.58%), respectively. Regarding the effect according to the type of vial, the efficiency and SQP(E) of both Ultima Gold LLT and Ultima Flo-AP showed the highest values in the order of teflon, polyethylene, and glass.

Tritium extraction in aluminum metal by heating method without melting

  • Kang, Ki Joon;Byun, Jaehoon;Kim, Hee Reyoung
    • Nuclear Engineering and Technology
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    • v.54 no.2
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    • pp.469-478
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    • 2022
  • Tritium was extracted from tritium-contaminated aluminum samples by heating it in a high-temperature furnace at 200, 300, or 400 ℃ for 15 h. The extracted tritium was analyzed by using a liquid scintillation counter (LSC); the sample thicknesses were 0.4 and 2 mm. The differences in tritium extraction over time were also investigated by cutting aluminum stick samples into several pieces (1, 5, 10, and 15) with the same thickness, and subsequently heating them. The results revealed that there are most of the hydrated material based on tritium on the surface of aluminum. When the temperature was increased from 200 or 300 ℃-400 ℃, there are no large differences in the heating duration required for the radioactivity concentration to be lower than the MDA value. Additionally, at the same thickness, because the surface of aluminum is only contaminated to tritiated water, cutting the aluminum samples into several pieces (5, 10, and 15) did not have a substantial effect on the tritium extraction fraction at any of the applied heating temperatures (200, 300, or 400 ℃). The proportion of each tritium-release materials (aluminum hydrate based on tritium) were investigated via diverse analyses (LSC, XRD, and SEM-EDS).

A Study on the Changes of Taste Components in brisket and shank Gom-Kuk by Cooking Conditions (조리조건에 따른 양지머리와 사골곰국의 맛성분 변화에 대한 연구)

  • 조은자;정은정
    • Korean journal of food and cookery science
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    • v.15 no.5
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    • pp.490-499
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    • 1999
  • The purpose of this study was to investigate the changes of taste components in the boiled beef brisket soup stock and shank soup stock by varying pretreatment, boiling temperature and time. Free amino acids and nucleotides color and sensory evaluation in each samples were analyzed. The results were obtained as follows : 1. The amount of free amino acids in the brisket soup stock pretreated by soaking and blanching showed a tendency to increase in proportion to boiling time. The amount of glutamic acid in the brisket soup stock was much in order of soaking > blanching > roasting pretreatment. While the amount of glutamic acid in the boiled soup stock samples pretreated by soaking and blanching was much more at low temperature than at high temperature, the glutamic acid contents in the boiled soup stock pretreated by roasting were large at high temperature. The amount of glutamic acid in pretreated by soaked soup stock showed the highest and recorded 8.73 mg% at 6 hour-low temperature-boiling. 2. The amount of free amino acids in the shank soup stock did not show any regular tendency and had few changes in quantity by the methods of pretreatment. Each amount of glutamic acid in the shank soup stock pretreated by soaking and blanching was the highest, when boiled for 3 hours at high temperature. The samples pretreated by roasting showed the highest record 2.49 mg%, when boiled for 6 hours at high temperature, but could not recognize any regular tendency in the case of boiling at low temperature. 3. The amount of nucleotides in the brisket soup stock generally showed increase in proportion to boiling time. The amount of 5'-IMP extracted from the brisket soup stock was much in order of blanching > soaking > roaking pretreatment, but few differences between blanching and soaking soup stock samples. The amount of 5'-IMP extracted from soup stock samples pretreated by soaking and blanching was high at low-boiling and by roasting at high-boiling. Each amount of 5'-IMP extracted from soup stocks pretreated by soaking(BSL) and blanching(BBL) was the highest at 6 hour-low-boiling(37.06 mg%), and 5 hours(38.37 mg%) respectively. The amount of 5'in the soup stock pretreated by roasting(BRH) showed the highest records at 6 hour-high-boiling(10.85 mg%). 4. The amount of 5'-IMP extracted from the shank soup stock preteated by soaking and blanching showed a tendency to decrease after 3 hours boiling irrelative of boiling temperature. The amount of 5'in the shank soup stock was much in order of soaking > blanching > roasting pretreatment and showed high at the boiling of high temperature. In the sample pretreated by roasting it showed the highst records when boiled for 6 hours at high temperature(1.55 mg%). 5. The L Value of the brisket soup stock pretreared by roasting at high temperature(BRH) was the lowest and the b value of it was the highest of all the brisket samples boiled for 6 hours. No differences were found in the Value of L, a, and b in shank soup stock by the methods of pretreatment and boiling temperature. 6. The sensory scores in color and flavor of the brisket soup stock showd that BRH was higher than the other samples, and the preference in taste and overall was the highest in BSH while it was the lowest in BRH. The preference in the all sensory characteristics of SSH was higher than any other shank soup stock, but did not show any significant difference statistically.

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Effects of Physical and Chemical Treatment as the Pretreatments on Microorganisms and Quality Characteristics of Allium monanthum (전처리 방법이 달래의 품질 특성과 미생물 저감에 미치는 영향)

  • Shim, Hyun-Jeong;Seong, Ok-Lan;Cho, Yong-Sik;Jang, Hyun-Wook;Hwang, Young
    • Journal of Food Hygiene and Safety
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    • v.36 no.6
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    • pp.510-519
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    • 2021
  • The purpose of this study was to investigate the effect of the microbial reduction and quality maintenance of the physical and chemical pretreatment of Allium monanthum. For physical treatment, handwash, bubble wash and ultrasonication were conducted at 50℃ and 60℃ for 1, 3 and 5 minutes, respectively, and for chemical treatment the sample was immersed in fumaric acid and acetic acid of 1.5% and 2% concentrations for 1, 3 and 5 minutes, respectively. As a result of the microorganism and quality analysis, 3 minutes of bubble wash was the most effective physical pretreatment in reducing fungi although the effect on reducing total viable bacterial was small. Furthermore, 5 minutes of ultrasonication at 60℃ significantly reduced microorganisms, but also resulted in the reduction of the a value of chromaticity, which cause the green color to fade. With chemical pretreatment, it was found that treating with fumaric acid was more effective in reducing the total viable bacteria and fungi than acetic acid. The result shows that 1.5% concentration of fumaric acid is the most effective with 3 minutes of treatment time. The quality of Allium monanthum were compared in the combination of the two most effective microorganism reduction pretreatments: 3 minutes of bubble wash (B3) and 3 minutes in 1.5% fumaric acid (F153). As a result of analyzing the quality characteristics over 9 days of storage at 4℃ after the treatments, it was revealed that the BF treatment is more effective in reducing fungi than the total viable bacteria. The results shows that the BF treatment is more effective in reducing total viable bacteria, whereas the F153 treatment is more effective in reducing fungi. Also, it was found that the 𝚫E value in BF was the lowest, whereas F153 treatment showed the green color faded. The maximum cohesiveness changed more significantly in the green stems than in the roots. On the 9th day of storage, the hardness of the green stem was found to be maintained at the highest level (P<0.05) after F153 treatment, whereas that of the roots decreased (P<0.05) since the 6th day after the bubble wash. Considering the reduction of microorganisms and the quality maintenance of Allium monanthum, the most effective pretreatment methods were 3 minutes in 1.5% fumaric acid for reducing microorganisms and maintaining color and maximum cohesiveness, and the combined process could also be effective if the expiration period is within 3 days.

Experimental Study on the Influence of the Function of Spleen on Learning and Memory (비기능이 학습과 기억에 미치는 영향에 대한 실험적 연구)

  • 박찬원;이진우;채한;홍무창;신민규
    • The Journal of Korean Medicine
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    • v.20 no.4
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    • pp.39-49
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    • 2000
  • This study was conducted to prove that there exists a relation between the spleen and learning and memory as Oriental medicine believesTo promote the function of the Spleen, Guibitang was administered to rats in this study. Rats were 250~300g Sprague-Dawley, and were divided into three groups. One was the normal group without any pretreatment. Another was the control group which was administered normal saline and the abdominal injection of L-NAME before learning and memory test. And the 3rd was the sample group, to which was administered Guibitang extract and (no 'the') abdominal injection of L-NAME before the learning and memory test. Each group was made up of 12 rats. Morris water maze and radial arm maze tasks were performed in the learning test and Morris water maze task in the memory test. For 2 days to evaluate the ability of learning in the Morris water maze, 16 trials were carried out and first latency(lapse time to find the escape platform for the first time) was measured. The next day, to evaluate the ability of memory, the escape platform was eliminated from the maze, and total path, target entry number, first latency and memory score were measured. 48hrs before the radial arm maze task was performed, bait was deprived from each group. After learning test, bait was permitted to each group. So 85% of the body weight was maintained for 6 days of the test. Each of the eight arms was baited; correct choice numer and error were counted; each trial was finished when the rat had entered each of the eight arms, or more than 10 minutes had elapsed. The results were as follows: In the learning test, the first latency of the sample group in the Morris water maze showed evident improvement of learning compared to control group at the 11th, 12th, 13th trial of 16 trials, and correct choice number in radial arm maze showed noticeable improvement compared to the control group at 3rd, 4th and 5th; In the memory test, the memory score of the sample group showed evident improvement compared to the control group. From the above results, the administration of Guibitang, which tonifies the function of the Spleen, could enhance the ability of learning and memory. So it was suggested that the Spleen has a relation with learning and memory.

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Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector (고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석)

  • Hong, Jee-Eun;Kim, Mi-Ran;Cheon, Sang-Hee;Chai, Jung-Young;Park, Eun-Ryong;Mun, Chun-Sun;Gwak, In-Shin;Kim, Ok-Hee;Lee, Kwang-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.3
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    • pp.359-363
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    • 2009
  • This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area ($r^2$=1.000) in the range of $0.02{\sim}10.0$ mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of $53.5{\sim}140.3$ mg/kg.

A Protocol of Ludox Treatment for Physiological and Molecular Biological Research of Freshwater Cyanobacteria (퇴적층 남조류 휴면세포의 생리적-분자생물학적 연구를 위한 Ludox 처리법)

  • Keonhee Kim;Kyeong-eun Yoo;Hye-in Ho;Chaehong Park;Hyunjin Kim;Soon-Jin Hwang
    • Korean Journal of Ecology and Environment
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    • v.56 no.1
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    • pp.94-103
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    • 2023
  • Cyanobacterial resting cells, such as akinetes, are important seed cells for cyanobacteria's early development and bloom. Due to their importance, various methods have been attempted to isolate resting cells present in the sediment. Ludox is a solution mainly used for cell separation in marine sediments, but finding an accurate method for use in freshwater is difficult. This study compared the two most commonly used Ludox methods (direct sediment treatment and sediment distilled water suspension treatment). Furthermore, we proposed a highly efficient method for isolating cyanobacterial resting cells and eDNA amplification from freshwater sediments. Most of the resting cells found in the sediment were akinete to the Nostocale and were similar to those of Dolichospermum, Cylindrospermum, and Aphanizomenon. Twenty times more akinetes were found in the conical tube column using the sediment that had no treatment than in the sample treated by suspending the sediment in distilled water. Akinete separated through Ludox were mainly spread over the upper and lower layers in the column rather than concentrated at a specific depth in the column layer. The mibC, Geo, and 16S rDNA genes were successfully amplified using the sediment directly in the sample. However, the amplification products of all genes were not found in the sample in which the sediment was suspended in distilled water. Therefore, 5 g to 10 g of sediment is used without pretreatment when isolating cyanobacterial resting cells from freshwater sediment. Cell isolation and gene amplification efficiency are high when four times the volume of Ludox is added. The Ludox treatment method presented in this study isolates cyanobacterial resting cells in freshwater sediment, and the same efficiency may not appear in other biotas. Therefore, to apply Ludox to the separation of other biotas, it is necessary to conduct a pre-experiment to determine the sediment pretreatment method and the water layer where the target organism exists.