• Title/Summary/Keyword: Formic Acid

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Thermotropic and Lyotropic Liquid Crystalline Behavior of N,O-Hydroxypropyl Chitosans (N,O-히드록시프로필 키토산들의 열방성과 유방성 액정 거동)

  • Kim, Hyo-Gap;Jung, Seung-Yong;Ma, Yung-Dae
    • Polymer(Korea)
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    • v.36 no.3
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    • pp.380-392
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    • 2012
  • Four kinds of N,O-hydroxypropyl chitosans (HPCTOs) with degree of substitution(DS) and molar substitution (MS) ranging from 2.47 to 2.52 and 4.9 to 7.8, respectively were synthesized, and their molecular chracteristics and thermotropic and lyotropic liquid crystalline properties were investigated. MS was exceedingly larger than DS, showing that in the later stages of reaction, propylene oxide was preferentially added to the side chains rather than the main chain. All the derivatives formed thermotropic cholesteric phases. The glass and clearing temperatures were decreased with increasing MS. The optical pitches (${\lambda}_m$'s) of the thermotropic cholesteric phases increased with temperature. However, the ${\lambda}_m$'s of the derivatives at the same temperature increased with increasing MS. Solutions of HPCTOs in water, methanol, ethanol, acetic acid, and formic acid containing more than 30 wt% polymer also formed cholesteic phases whose ${\lambda}_m$'s decreased exponentially with increasing polymer concentration. The concentration dependence of ${\lambda}_m$ of HPCTO solutions, however, highly depended on the nature of the solvent and MS. The thermotropic and lyotropic mesophase properties of HPCTOs were significantly different from those reported for hydroxypropyl celluloses. The results indicate that the secondary amino group in the C-2 position plays an important role on the formation, stabilization, and temperature and concentration dependencies of ${\lambda}_m$ of the cholesteric mesophase.

Screening of Antithrombotic Peptides from Soybean Paste by the Microplate Method (Microplate법에 의한 된장유래의 항혈전 펩타이드 탐색)

  • Shon, Dong-Hwa;Lee, Kyung-Ae;Kim, Seung-Ho;Ahn, Chang-Won;Nam, Hee-Sop;Lee, Hyung-Jae;Shin, Jae-Ik
    • Korean Journal of Food Science and Technology
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    • v.28 no.4
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    • pp.684-688
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    • 1996
  • In order to search for antithrombotic peptides from soybean paste, the inhibitory activity of water extract of soybean paste and its peptide fractions on ADP-induced aggregation of washed platelets was assayed. Soybean paste extract treated with ultrafiltration (M.W. cut off, 3,000 daltons) was found to have inhibitory activity of 90% at the dose of $96\;{\mu}g/ml$ by the method of turbidometric aggregometer. Soybean paste extract was fractionated to 19 fractions (No. B-18) by Dowex 50W X-2 ion exchange column chromatography and activity test was performed by the microplate method. All of the fractions had antithrombotic activity $(IC_{50},\;101,000\;{\mu}g/ml)$, and most fractions had higher activity than positive control, RGDS $(IC_{50}.\;205\;{\mu}g/ml)$. Especially, basic fractions No.16-18 showed higher activity than soybean paste extract $(IC_{50},\;30\;{\mu}g/ml)$. The fraction No.16 with the highest activity $(IC_{50},\;10\;{\mu}g/ml)$ was purified and analysed for amino acid composition. The results showed that histidine, arginine, and alanine were major residues in the peptide part of the fraction.

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Rapid and Simultaneous Determination of Ginsenosides Rb1, Rb2, Rc and Re in Korean Red Ginseng Extract by HPLC using Mass/Mass Spectrometry and UV Detection

  • Kwon, Young-Min;Lee, Sung-Dong;Kang, Hyun-Sook;Cho, Mu-Gung;Hong, Soon-Sun;Park, Chae-Kyu;Lee, Jong-Tae;Jeon, Byeong-Seon;Ko, Sung-Ryong;Shon, Hyun-Joo;Choi, Dal-Woong
    • Journal of Ginseng Research
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    • v.32 no.4
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    • pp.390-396
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    • 2008
  • For evaluating the quality of ginseng, simple and fast analysis methods are needed to determine the ginsenoside content of the ginseng products. The aim of this study was therefore to optimize conditions for fast analysis of the ginsenosides, the active ingredients in extracts of Korean red ginseng. When tandem HPLC mass spectrometry (HPLC-MS/MS) was used, four forms of ginsenoside, Rb1, Rb2, Rc, and Re, were readily separated in seven minutes using a gradient mobile phase (acetonitrile and water containing acetic acid). This is the shortest separation time reported among the studies of major ginsenoside analysis. When gradient HPLC with UV detection was used, the detection limit was high, but separation of these four ginsenosides required 25 minutes using acetonitrile and water containing formic acid as a mobile phase. HPLC-MS/MS was able to separate ginsenoside Rg1 easily regardless of the mobile phase condition, but the HPLC-UV could not separate Rg1 because acetonitrile concentration in the mobile phase had to be maintained below 20%. Ginsenoside peaks were clearer and had more sensitive detection limits when Korean red ginseng extract was analyzed by the HPLC-MS/MS, but the UV detection was useful for chromatographic fingerprinting of all four major ginsenosides of the extract: Rb1, Rb2, Rc, and Re. Extracts were found to contain 2.17 mg, 1.51 mg, 1.29 mg, and 0.46 mg of ginsenoside Rb1, Rb2, Rc, Re, respectively, per gram weight. The ratios of each ginsenoside in the extracts were 1.0 : 0.7 : 0.6 : 0.2, respectively. Taken together, the results indicate that HPLC-MS/MS spectrometry could be the most useful method for rapid analysis of even small amounts of major ginsenosides, while HPLC with UV detection could also be used for rapid analysis of major ginsenosides and for quality control of ginseng products.

Wet Oxidation of Phenol with Homogeneous Catalysts (균일촉매를 이용한 페놀의 습식산화)

  • Suh, Il-Soon;Ryu, Sung Hun;Yoon, Wang-Lai
    • Korean Chemical Engineering Research
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    • v.47 no.3
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    • pp.292-302
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    • 2009
  • The wet oxidation of phenol has been investigated at temperatures from 150 to $250^{\circ}C$ and oxygen partial pressures from 25.8 to 75.0 bar with initial pH of 1.0 to 12.0 and initial phenol concentration of 10 g/l. Chemical Oxygen Demand COD has bee measured to estimate the oxidation rate. Reaction intermediates have been identified and their concentration profiles have been determined using liquid chromatography. The destruction rate of phenol have shown the first-order kinetics with respect to phenol and the changes in COD during wet oxidation have been described well with the lumped model. The impact of various homogeneous catalysts, such as $Cu^{2+}$, $Fe^{2+}$, $Zn^{2+}$, $Co^{2+}$ and $Ce^{3+}$ ions, on the destruction rate of phenol and COD has also been studied. The homogeneous catalyst of $CuSO_4$ has been found to be the most effective for the destruction of phenol and COD during wet oxidations. The destruction rate of formic acid formed during wet oxidations of phenol have increased as increasing temperature and $CuSO_4$ concentration. The final concentrations of acetic acid which has been formed during wet oxidations and difficult to oxidize have increased with reaction temperature and with decrease in the catalyst load.

Effect of Thermal Treatments on Flavonoid Contents in Domestic Soybeans (국내산 대두(Glycine max. Merr)자원의 플라보노이드 대사체 동정 및 열처리 효과)

  • Shin, Jae-Hyeong;Kim, Heon-Woong;Lee, Min-Ki;Jang, Ga-Hee;Lee, Sung-Hyen;Jang, Hwan-Hee;Hwang, Yu-Jin;Park, Keum-Yong;Song, Beom-Heon;Kim, Jung-Bong
    • Korean Journal of Environmental Agriculture
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    • v.34 no.2
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    • pp.105-110
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    • 2015
  • BACKGROUND: Soy isoflavones, structurally similar to endogenous estrogens, may affect human body through both hormonally mediated and non-hormonally related mechanisms. Heat processing could change chemical compositions. The effects of different thermal processes, boiling and HTHP(high temperature and high pressure) on the composition of isoflavone compounds and total amount of domestic soybeans were investigated in this study. METHOD AND RESULTS: Three different kinds of soybean samples were collected from RDA-Genebank. The samples were extracted using methanol, distilled water, and formic acid based solvent. Also the same solvents were used for mobile phase in UPLC/ToF/MS. All of the isoflavone compounds were analyzed based on the aglycone type of external standard for quantification. The standard calibration curve presented linearity with the correlation coefficient R2 > 0.98, analysed from 1 to 50 ppm concentration. The total isoflavone contents does not change by treatment within the same breed. While "boiling" and "HTHP" processes tend to increase the contents of aglycone and ${beta}$-glucosides, "fresh" soybeans retained the high concentration of malonylglucosides. CONCLUSION: These results have to be considered while developing an effective functional food, from the health while point of view using soybeans.

Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry (LC-MS/MS를 이용한 수산물 중 콜리스틴 분석법 개발)

  • Shin, Dasom;Kang, Hui-Seung;Lee, Soo-Bin;Cho, Yoon-Jae;Cheon, So-Young;Jeong, Jiyoon;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.319-326
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    • 2016
  • Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with $r^2$ > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.

Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Validation of an LC/MS/MS Method for the Pharmacokinetic Study of Lercanidipine (염산레르카니디핀 체내동태 연구를 위한 혈청 중 레르카니디핀의 LC/MS/MS 정량법 검증)

  • Kim, Se-Mi;Kim, Hwan-Ho;Shin, Sae-Byeok;Kang, Hyun-Ah;Yoon, Hwa;Cho, Hea-Young;Kim, Yoon-Gyoon;Yang, Chan-Woo;Yong, Chul-Soon;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.37 no.4
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    • pp.223-227
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    • 2007
  • A rapid, simple and sensitive LC/MS/MS method for the determination of lercanidipine in human serum was validated and applied to the pharmacokinetic study of lercanidipine. Lercanidipine and internal standard, amlodipine, were extracted from human serum by liquid-liquid extraction with hexan-isoamyl alcohol (100: 1, v/v) and analyzed on a $Symmetry^{(R)}$ MS $C_{18}$ column with the mobile phase of acetonitrile-0.2% aqueous formic acid (70: 30, v/v). Using MS/MS with multiple reaction monitoring (MRM) mode, lercanidipine and amlodipine were detected without severe interferences from human serum matrix. Lercanidipine produced a protonated precursor ion ($[M+H]^+$) at m/z 612.3 and a corresponding product ion at m/z 280.0. Internal standard produced a protonated precursor ion ($[M+H]^+$]) at m/z 409.0 and a corresponding product ion at m/z 238.0. The ruggedness of this method was investigated using quality control (QC) samples. This method showed linear response over the concentration range of 0.05-20 ng/mL with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 mL of serum was 0.05 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the developed method ranged from 85.51 to 112.2% for lercanidipine with overall precision (% C.V.) being 3.56-13.1%. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of lercanidipine in human serum samples for the pharmacokinetic studies, demonstrating the suitability of the method.

Damage Characteristics of Korean Traditional Textiles by Formaldehyde (포름알데히드에 의한 전통직물의 손상 특성)

  • Kim, Myoung Nam;Lim, Bo A;Lee, Sun Myung
    • Journal of Conservation Science
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    • v.30 no.4
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    • pp.353-364
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    • 2014
  • Formaldehyde(HCHO) may have a damage effect on Korean traditional textiles, because concentration is high and occurrence frequency is frequent at the exhibition room and storage area. Total 20 specimens were prepared using 4 different materials (silk, cotton, ramie, hemp) after dyeing with 5 colors (undyed, red, yellow, blue, black). The specimens were exposed to HCHO gas in the test chamber. The gas acceleration test was conducted to identify the deterioration of Korean traditional textiles according to HCHO concentration(0.5, 1, 10, 100, 500ppm), to temperature-humidity condition at HCHO 500ppm, and deterioration conditions at HCHO 500ppm. Optical, chemical, and physical evaluation was carried out after the exposure. The results, color difference, grey scale rating, formate($HCO_2{^-}$) of some textiles increased at 500ppm, while pH decreased at 500ppm. Also, color difference, grey scale rating, formate($HCO_2{^-}$) of some textiles increased double damage at high temperatures & humidity, high humidity condition. But, damages of accelerated degradation textiles were slight, because of degradation degree and degradation products. The results suggest that determined the damage to the korean traditional textile, damage level, damage-weighted condition, damage to accelerated degradation textiles. In addition, formaldehyde damaged to yellowing of red textiles, bleaching of accelerated degradation textiles, formic acid damaged to bleaching of total 20 specimens.

Body Residue-based Approach as an Alternative of the External Concentration-based Approach for the Ecological Risk Assessment (외부환경농도에 기반한 생태위해성 평가방법의 대안으로서 생체잔류량 접근법)

  • Lee Jong-Hyeon
    • Environmental Analysis Health and Toxicology
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    • v.21 no.2 s.53
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    • pp.185-195
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    • 2006
  • 환경오염물질로부터 수생태계 보호를 위한 표준적인 평가 및 관리 수단인 수질환경기준은 오염물질의 독성작용이 일어나는 표적기관에서의 오염물질의 농도에 대한 대체측정치로서 환경 내 오염물질의 농도를 이용해 왔다. 이러한 '외부환경농도에 기반한 접근방법'은 표적기관에서의 독성물질의 농도가 생물체내 농도에 비례하고, 결국 외부환경농도에도 비례할 것이라고 가정한다. 따라서 환경오염물질의 생물이용도나 생물축적 양상의 차이 때문에 고유 독성치를 비교 평가하는데 한계가 있다. 이와 달리 '생물체내 농도에 기반한 접근방법(이하 생체잔류량 접근법)'은 환경오염물질의 생물이용도나 종 특이적 생물축적 양상과 관련된 불확실성을 제거하고, 환경오염물질 고유의 독성을 비교 평가할 수 있게 해준다. 특히 생체잔류량 접근법을 독성동태학 및 독성역학 모델과 함께 사용하는 경우는 실제 현장에서 일어나는 복잡한 노출조건에서의 독성영향을 예측하는데 활용할 수 있다. '생체잔류량 접근법'은 독성기작별 임계잔류량(Critical Body Residue)을 결정함으로써 생물모니터링의 결과를 해석하는데 적용되고 있다. 또한 생태위해성평가를 위해서 필요한 '무영향예측농도(Predicted No-effect Concentration, PNEC)를 예측하기 위한 방법으로 생체 내 잔류량에 기반해서 농도-시간-반응관계를 기술하고, 예측할 수 있는 새로운 유형의 독성역학 및 독성동태학 모델을 제시하고, 생체내 '무영향농도(No Effect Concentration, NEC)'를 추정하게 해 준다. 특히 생체내 NEC는 '무영향관찰농도(No Observed Effect Concentration, NOEC)'와 '영향농도(Effect Concentration, EC)'처럼 분산분석이나 회귀분석모델과 같은 통계적 모델에 기반해서, 농도-반응관계만을 기술할 뿐인 기존 독성모델을 대체할 대안으로 최근에 OECD와 ISO에 의해서 추천되었다.분석을 시행한 결과 인지기능 장애정도 및 MMSEK 점수 증가에 따른 사망위험도는 어느 모형에서도 인지기능 장애정도가 사망에 미치는 위험도는 통계적으로 유의하지 않았다(표 6, 표 7). 이상 본 연구는 농촌지역 노인들에서 인지기능 장애정도가 사망에 미치는 영향을 알아보고자 하였지만, 인지기능 장애정도가 사망에 미치는 영향을 통계적으로 유의하게 고찰하지 못하였다.의한 차이를 보였다. (P<0.05, P<0.001) 5. Excelco로 부식처리된 도재가 5% HF 용액으로 부식처리된 도재보다 부식정도가 더 현저하였다.은 제언을 하고자 한다. 먼저, 학교급식에 대한 식단 작성 시 학생들이 학교에서 제공되기 원하는 식단에 대한 의견을 받고 그 의견에 대한 결과를 게시하여 학생들이 제공되기 원하는 식단을 급식 시 제공하여 학생들이 식단선택에 동참할 수 있는 기회를 주는 것이 바람직하겠다. 또한 영양사는 학급의 반대표와의 정기적인 모임을 가짐으로서 학생들의 불만사항 및 개선 요구사항에대해 서로 의견을 교환하여 설문지조사가 아닌 직접적인 대화를 하여 문제점을 파악하고자 하는 적극적인 자세가 필요하겠다. 특히 아침식사의 결식 빈도가 높았고 이는 급식성과에 부정적인 영향을 줄 뿐 아니라 학교에서 제공하는 음식의 섭취정도에도 영향을 주고 있으므로 학생들에게 학부모와 전담교사 및 학교영양사는 학생들에게 이상적인 아침식사에 대한 교육은 물론이고 아침식사를 실천할 수 있도록 다양한 방안에 대해 함께 연구해야 하겠다. 정부차원에서 학교급식에 아침식사 프로그램을 도입할 수 있는 방안을 연구하고, 아침을 결식하는 학생이 학교에서 수업시작 하기 전에 간단한 식사를 할 수 있는 정책 도입이 필요하다acid의 생성량(生成量)을 측정(測定)하였는데 periodate의 소비량(消費量)은 1.23 mole, formic acid의 생성량(生成量)은 0.78 mole이다.한 경우도 비교적 많이 먹고 있었다(24.3%). 남 여