• Title/Summary/Keyword: organic acid chromatography

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Development of HPLC-UV method for detection and quantification of seven organic acids in animal feed (사료 중 유기산 7종 동시분석법 개발 및 유통 사료의 모니터링)

  • Kim, Jin kug;Lee, Mi Jin;Lee, Ye Ji;Kim, Hye Jin;Jeong, Min Hee;Kim, Ho Jin
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.202-208
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    • 2016
  • 본 연구에서는 사료 첨가제로 이용되고 있는 유기산 7종(formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid, propionic acid)의 동시분석법 개발을 위한 연구를 실시하였다. 7종의 화합물은 표준물질의 Retention time과 UV spectra를 통해 구별하였고, 분석법 검증은 직선성, 민감성, 선택성, 정확성, 정밀성을 통하여 검증하였다. 그 결과로 LOD와 LOQ의 범위가 각각 43~26,755 μg/kg, 12-8,026 μg/kg으로 설정하였고, 평균 회수율이 79.3~95.2%로 우수하게 보였으며, intra-day, inter-day에 대한 전반적인 상대 표준 편차(%RSD)는 3.2% 미만으로 나타났다. 이와 같이 검증된 자료를 통해 유기산의 동시분석에 대한 직선성, 민감성, 선택성, 정확성 및 정밀성을 확인하였고, 높은 수준을 나타냄을 알 수 있었다. 이를 바탕으로 유기산이 검출되는 단미사료 46 가지를 분석에 적용하여 진행하였고, 정량과 동시분석 검출을 위한 방법은 RP-HPLC/UV 검출기를 이용하여 성공적으로 개발되었다. 따라서 본 연구결과를 바탕으로 하여 사료 중의 유기산의 분석이 신속하고 정확해졌을 뿐 아니라, 다른 종류의 사료 또한 이를 적용하여 효율적으로 이용할 수 있을 것으로 판단된다.

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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Determination of sulfur containing organic drugs by means of thin layer chromatography and flask combustion method (Thinlayer chromatography및 oxygen combustion flask method에 의한 유기유황약품의 분리정량)

  • 백남호;김박광
    • YAKHAK HOEJI
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    • v.13 no.2_3
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    • pp.84-87
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    • 1969
  • Microanalysis of organic sulfur compounds by means of combining thin layer chromatography and oxygen combustion flask method was attempted. The following procedure was found to be very simple and to give accurate results. The mixture of sulfa drugs was separated with T.L.C., and it was burned in a flask filled with oxygen, and the gas formed was absorbed in a dilute solution of sodium hydroxide. The solution was neuralized with hydrochloric acid and heated in a water bath. The sulfate ion formed was then treated with barium chromate solution and its absorbancy at 370 m.mu. was measured.

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Analysis of secondary reactions in concentrated sulfuric acid hydrolysis of hollocellulose by 1H-NMR spectroscopy (1H-NMR 분광분석을 통한 진한 산 가수분해 반응 2차 반응 조건 분석)

  • Lee, Jai-Sung;Shin, Soo-Jeong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.46 no.3
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    • pp.37-43
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    • 2014
  • Kinetics of holocellulose hydrolysis in concentrated sulfuric acid was analyzed using $^1H$-NMR spectroscopy with different reaction time, temperature and acid concentration in secondary hydrolysis. In this work, reaction condition of secondary hydrolysis was similar to concentrated sulfuric acid process with electrodialysis or simulated moving bed chromatography process for sulfuric acid recycling. By $^1H$-NMR spectroscopy, acid hydrolyzates from higher secondary acid hydrolysis (25-35% acid concentration) was successfully analyzed without any difficulties in neutralization or adsorption of acid hydrolyzate to solid salt. Higher acid concentration, higher temperature and longer reaction time led to more cellulose for glucose conversion but accompanied with glucose to galactose isomerization, glucose to unknown compounds and degradation of glucose to organic acid via furans.

Organic acidemias in Korea - Eight years experience of organic acid analysis - (유기산혈증-유기산 분석 8년의 정리)

  • Bang, Jun Suck;Lim, Si Hong;Lee, Kyung Hwa;Bae, Eun Joo;Park, Won Il;Lee, Hong Jin
    • Clinical and Experimental Pediatrics
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    • v.49 no.3
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    • pp.258-267
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    • 2006
  • Purpose : We have done this retrospective study to know the relative incidence and clinical manifestations of organic acidopathies in Korea during 8 years(from Jul. 1997 to May 2005). This results of organic acid analysis of 1,787 patients were compared with the results of organic acid analysis that were published three years ago. Methods : The results of quantitative organic acid analysis of samples of 1788 patients, referred from Jul. 1997 to May 2005, were analyzed retrospectively according to four age group(-2 mon, 3 mon-2 years, 3-12 years) and major clinical manifestations. Quantification of 83 organic acids was done with gas chromatography and mass spectometry. Results : We diagnosed 470 patients with 27 diseases of organic acid metabolism during this study period. Diseases found more than 10 cases are cytosolic 3-ketothiolase deficiency, mitochondrial respiratory chain disorders, PDHC deficiency, mitochondrial 3-ketothiolase deficiency, glutaric aciduria type II, biotinidase deficiency, methylmalonic aciduria and propionic aciduria. Other diseases were diagnosed in less than 10 cases. Conclusion : Though the incidence of individual organic acidemia is low, the overall incidence of organic acidemia as a whole seems to be relatively high in Korea. Compared with the results of organic acid analysis that were reported three years ago, we couldn't find a new disease and the difference of the relative incidences of high incident diseases. We were apprehensive of the errors that was owing to the short study period(3 years), but the relative incidences of our study(8 years) were similar to the results of organic acid analysis that were reported three years ago.

Effects of Titratable Acidity and Organic Acids on Enamel Erosion In Vitro

  • Kim, Eun-Jeong;Jin, Bo-Hyoung
    • Journal of dental hygiene science
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    • v.19 no.1
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    • pp.1-8
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    • 2019
  • Background: Erosion is a gradual process that occurs fairly quickly, and the full extent of the erosive effects of acidic beverages is not yet clear. The present study aimed to determine the differences in the erosive potentials among four naturally acidic fruit nectars within the same range of titratable acidity and to determine the influence of the components of organic acids on tooth erosion. Methods: Diluted fruit nectars (mandarin 1:1.1, orange 1:1.7, lemon 1:15, grapefruit 1:20) with the same range of titratable acidity (7.9 ml) and their corresponding organic acids (0.05%, 0.1%, 0.3%, and 0.5% citric acid, malic acid, and a citric and malic acid mixture [pH 2.8], respectively) were used. Specimens were placed in conical tubes with 50 ml of each of the test solutions for 1 hour. A microhardness test and scanning electron microscopy were used to measure enamel erosion. Acid separation was carried out using high-performance liquid chromatography to analyze the composition of each test solution. Results: Similar decreases in the Vickers hardness number (VHN) were observed among the groups treated with the following diluted fruit nectars: diluted mandarin nectar ($75.9{\Delta}VHN$), diluted lemon nectar ($89.1{\Delta}VHN$), diluted grapefruit nectar ($91.7{\Delta}VHN$), and diluted orange nectar ($92.5{\Delta}VHN$). No statistically significant differences were found in the enamel surface hardness after erosion (p>0.05). Citric and malic acids were the major organic acids in the test fruits. The lemon and orange groups had the highest malic acid concentrations, and the mandarin group had the lowest malic acid concentration. Conclusion: The titratable acidity and the citric and malic acid contents of the fruits could be crucial factors responsible for enamel erosion. Therefore, fruit-based drinks should be regarded as potentially erosive.

Recovery and Characterization of Lactic Acid from Fermentation Broth Using Chemical Precipitation (화학침전을 이용한 발효액의 젖산 회수 및 유기물 특성분석)

  • Lee, Wontae
    • Journal of the Korea Organic Resources Recycling Association
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    • v.26 no.1
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    • pp.47-53
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    • 2018
  • Recovery of lactic acid from fermentation broth using chemical precipitation was investigated with various chemicals. Effects of chemical types, mixing speeds, settling duration, and solvent addition were evaluated to improve the recovery rates of lactic acid. Overall, recovery efficiencies increased as the dosage of chemicals increased. Recovery rate of lactic acid by CaO was higher than those of $Ca(OH)_2$ and $CaCO_3$. Recovery of lactic acid increased by 48% under the optimized reaction conditions which included a mixing speed at 180 rpm, a settling duration of 24 h, and addition of ethanol at 25%(v/v). Practical application needs to consider types and concentrations of other organic acids as well as lactic acid. Based upon the results of fluorescence excitation emission matrix (FEEM), size exclusion chromatography (SEC), characteristics of recovered lactic acid were same as that in the fermentation broth.

Simultaneous Determination of Anthraquinone, Flavonoids, and Phenolic Antidiabetic Compounds from Cassia auriculata Seeds by Validated UHPLC Based MS/MS Method

  • Girme, Aboli;Saste, Ganesh;Chinchansure, Ashish;Joshi, Swati;Kunkulol, Rahul;Hingorani, Lal;Patwardhan, Bhushan
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.82-89
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    • 2020
  • A systematic isolation and characterization study for Cassia auriculata (CA) seeds resulted in identifying antidiabetic compounds 1,3,8-trihydroxyanthraquinone and quercetin, quercetin-3-O-rutinoside, gallic acid, caffeic acid, ferulic acid, and ellagic acid. The ultra-high-performance liquid chromatography based triple quadrupole mass spectrometry methodology was developed and validated for simultaneous identification and confirmation of these compounds from CA seeds. Multiple reaction monitoring (MRM) based quantification method was developed with MRM optimizer software for MS1 and MS2 mass analysis. The method was optimized on precursor ions and product ions with the ion ratio of each compound. The calibration curves of seven bioactive analytes showed excellent linearity (r2 ≥ 0.99). The quantitation results found precise (RSD, < 10 %) with good recoveries (84.58 to 101.42%). The matrix effect and extraction recoveries were found within the range (91.66 to 102.11%) for the CA seeds. This is the first MS/MS-based methodology applied to quantifying seven antidiabetic compounds in CA seeds and its extract for quality control purposes.

Investigation of toxic organic solvent exposure in work places (작업장에서의 유해 유기용제 폭로에 관한 연구)

  • Jo, Young Min;Kang, Sang Wan;Oh, Jong Min
    • Journal of Environmental Impact Assessment
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    • v.9 no.1
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    • pp.75-86
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    • 2000
  • The purpose of this work was to document the conditions regarding organic solvent exposure to the workers in paint industry. Air concentrations of organic solvents were measured by passive personal samplers and analyzed by a gas chromatography. Urine samples for hippuric test were also taken from 330 workers who have worked at seven domestic factories for more than two years. Amongst 25 organic elements detected in the indoor environment of working places, toluene was the most common element, and methanol showed the highest mean concentration(18.2ppm). A few elements including methylethyl ketone and toluene partially exceeded the Korean Permissible Exposure Limit. A lack of environmental facilities such as exhaust ventilation, automatic cleaning system, and personal safety devices at present work plaus brings about various occupational diseases.

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Organic acid and sugar contents in different domestic fruit juices

  • Kim, Young-Min;Hwang, So-Jeong;Seo, Mi-mi;Jin, So-Ra;Lee, Ki-Teak
    • Korean Journal of Agricultural Science
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    • v.43 no.5
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    • pp.705-714
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    • 2016
  • Organic acid and sugar contents in ten kinds of juices (two orange juices, two grape juices, two aloe juices, two citron juices, one bokbunja, and one grapefruit juice) were analyzed by high-performance liquid chromatography. Citric acid was detected in all the fruit juices analyzed. Grape juices contained the highest tartaric acid content (67.85 - 99.37 mg/100 mL) while orange and grape juices contained a high content of malic acid (151.67 - 211.18 mg/100 mL). Lactic acid was detected in all the aloe juices (35.12 - 65.27 mg/100 mL) as well as in one orange (203.8 mg/100 mL) and one grape juice (112.28 mg/100 mL). Citrus fruit juices (A, A', F) showed the highest content of total organic acids as 902.81 - 1,103.7 mg/100 mL. With regard to sugar contained in the juices, lactose and maltose were not detected in any of the fruit juices. Even when comparing the same kind of fruit juice, sugar (fructose, glucose, and sucrose) content showed a significant difference (p < 0.05) depending on the manufacturer. In the grape juices, contents of fructose (6.86 - 7.51) and glucose (6.23 - 7.3 g/100 mL) were higher than in other juices. One serving size of the juices (180 mL) analyzed in this study can provide approximately 3.3 - 4.9% of total daily energy requirements when consumed as part of the 2,200 kcal/day diet required for an adult.