• Title/Summary/Keyword: HPLC-analysis

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폴리올레핀계 포장재 중의 항산화제 분석 (Determination of Antioxidants in Polyolefin Packaging Materials)

  • 이근택;박영주
    • 한국포장학회지
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    • 제1권1호
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    • pp.20-28
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    • 1995
  • 폴리올레핀계 포장재에 첨가된 항산화제를 분석하기 위하여 Soxhlet 추출과 HPLC에 의한 분석방법을 검토하였다. Soxhlet에 의한 폴리올레핀계 포장재에서의 첨가제 추출은 약 10시간 이내에 거의 완료되는 것으로 나타났다. 또한 BHT, Irganox 1076, Irganox 1010, Irgafos 168 등 4가지 항산화제의 동시검색은 역상 HPLC를 이용하여 gradient elution으로 baseline resolution의 분리가 가능하였다. 또한 LLDPE와 OPP 필름 중에 첨가된 4가지 항산화제의 확인 및 정량도 가능하였다.

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Discrimination of Panax ginseng Roots Cultivated in Different Areas in Korea Using HPLC-ELSD and Principal Component Analysis

  • Lee, Dae-Young;Cho, Jin-Gyeong;Lee, Min-Kyung;Lee, Jae-Woong;Lee, Youn-Hyung;Yang, Deok-Chun;Baek, Nam-In
    • Journal of Ginseng Research
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    • 제35권1호
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    • pp.31-38
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    • 2011
  • In order to distinguish the cultivation area of Panax ginseng, principal component analysis (PCA) using quantitative and qualitative data acquired from HPLC was carried out. A new HPLC method coupled with evaporative light scattering detection (HPLC-ELSD) was developed for the simultaneous quantification of ten major ginsenosides, namely $Rh_1$, $Rg_2$, $Rg_3$, $Rg_1$, Rf, Re, Rd, $Rb_2$, Rc, and $Rb_1$ in the root of P. ginseng C. A. Meyer. Simultaneous separations of these ten ginsenosides were achieved on a carbohydrate analytical column. The mobile phase consisted of acetonitrile-water-isopropanol, and acetonitrile-water-isopropanol using a gradient elution. Distinct differences in qualitative and quantitative characteristics for ginsenosides were found between the ginseng roots produced in two different Korean cultivation areas, Ganghwa and Punggi. The ginsenoside profiles obtained via HPLC analysis were subjected to PCA. PCA score plots using two principal components (PCs) showed good separation for the ginseng roots cultivated in Ganghwa and Punggi. PC1 influenced the separation, capturing 43.6% of the variance, while PC2 affected differentiation, explaining 18.0% of the variance. The highest contribution components were ginsenoside $Rg_3$ for PC1 and ginsenoside Rf for PC2. Particularly, the PCA score plot for the small ginseng roots of six-year old, each of which was light than 147 g fresh weight, showed more distinct discrimination. PC1 influenced the separation between different sample sets, capturing 51.8% of the variance, while PC2 affected differentiation, also explaining 28.0% of the variance. The highest contribution component was ginsenoside Rf for PC1 and ginsenoside $Rg_2$ for PC2. In conclusion, the HPLC-ELSD method using a carbohydrate column allowed for the simultaneous quantification of ten major ginsenosides, and PCA analysis of the ginsenoside peaks shown on the HPLC chromatogram would be a very acceptable strategy for discrimination of the cultivation area of ginseng roots.

HPLC-CAD에 의한 산양삼의 극성 및 비극성 ginsenoside 동시 분석 (Simultaneous Analysis Method for Polar and Non-polar Ginsenosides in Cultivated Wild Ginseng by Reversed-phase HPLC-CAD)

  • 옥선;강재선;김강민
    • 생명과학회지
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    • 제26권2호
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    • pp.247-252
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    • 2016
  • 산양삼은 식품 또는 약초로써 많이 사용되고 있다. 이번 연구의 목표는 high performance liquid chromatography (HPLC) - charged aerosol detection (CAD)에 의해 산양삼의 추출물에 사포닌들의 분석을 최적화 하는 것이다. CAD는 물리적인 특성은 물론이고 입자크기, 스펙트럼 특성과는 무관하게 비휘발성 물질도 분석할 수 있다. 산양삼 추출물 중 Gensenoside Rb1, Rd, Rg1, Rf, Re 및 Rh1을 분석하였다. HPLC-CAD분석을 위한 사포닌 추출물은 건조 산양삼 10 g에 95% 에탄올 100 ml을 넣어 80℃에서 24시간 동안 추출하여 사포닌을 얻었다. 6개의 주요한 사포닌을 정량화하였을 경우 값은 다음과 같다. 사포닌들의 함량은 Rb1 (5.48±0.12 mg/g), Rd (5.33±0.14 mg/g), Rg1 (12.80±0.05 mg/g), Rf (19.08±0.68 mg/g), Re (19.87± 0.05 mg/g), 및 Rh1 (16.47±0.16 mg/g)로 확인하였다. 대체적으로 산양삼 추출물의 사포닌은 protopanaxatriol (Rg1, Rf, Re, Rh1)의 값이 protopanaxadiol (Rb1, Rd)보다 높게 확인 되었다. 이번 연구에서는 산양삼 사포닌의 분석조건을 HPLC-CAD를 이용하여 최적화하였고 제품화를 위해 약리활성에 관한 연구도 매우 중요할 것이다.

1H-NMR and HPLC analysis on the chiral discrimination of β-blockers using (S)-2-tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid

  • Seo, Sang Hun;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Kim, Kyeong Ho
    • 분석과학
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    • 제34권1호
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    • pp.9-16
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    • 2021
  • In the group of commonly prescribed β-blocker drugs, one of the enantiomers is generally relatively more active than the others. This study aims to develop a technique for the chiral analysis of select β-blockers based on proton nuclear magnetic resonance (1H-NMR) spectrometry. (S)-2-Tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid ((S)-TBMB) was synthesized and utilized as a chiral derivatizing agent. Pure β-blocker enantiomers were isolated from racemates by semi-preparative liquid chromatography prior to derivatization. The reaction time and concentration of (S)-TBMB were controlled to improve the derivatization procedure. No racemization was found during the analysis. High-performance liquid chromatography (HPLC) analysis was also performed for comparative purposes. High agreement between the NMR and HPLC methods was achieved in the determination of (R)-metoprolol in a standard solution of the (S) isomer.

누에에 함유된 1-Deoxynojirimycin의 분석을 위한 HPLC-ELSD 분석법 밸리데이션 (Development and Validation of a Unique HPLC-ELSD Method for Analysis of 1-Deoxynojirimycin Derived from Silkworms)

  • 조혜진;이설림;신명숙;이주환;이상현
    • 생약학회지
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    • 제54권1호
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    • pp.38-43
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    • 2023
  • A simple and accurate assay was developed for the quantitative analysis of 1-deoxynojirimycin (1-DNJ) derived from the silkworm (Bombyx mori). Normal-phase high-performance liquid chromatography coupled with an evaporative light scattering detector (HPLC-ELSD) and a hydrophilic interaction liquid chromatography column was used. Various parameters were applied to optimize the analysis method. The limits of detection and quantification of 1-DNJ were 2.97 × 10-3 and 9.00 × 10-3 mg/mL, respectively. The calibration curve showed good linearity results. The concentration range and the r2 value were 0.0625-1.0 mg/mL and 0.9997, respectively. The accuracy test demonstrated a significantly high recovery rate (89.95-103.22%). The relative standard deviation was ≤ 1.00%. Thus, a method for the accurate identification and quantitative analysis of 1-DNJ in silkworms was developed. Moreover, in this procedure, the process of derivatization of 1-DNJ, which was required in previous experiments, could be eliminated. This technique may be actively utilized for the development of pharmaceuticals and health functional foods using 1-DNJ.

배양조류 및 댐 저수지 조체중 신경독소 Anatoxin-a, Saxitoxin류의 분석 및 수처리방안 (Analysis of Neurotoxins, Anatoxin-a, Saxitoxin in Algae Cultured and Algae in Dam Reservoir and its Water Treatment)

  • 김학철;최일환
    • 환경위생공학
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    • 제23권4호
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    • pp.37-44
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    • 2008
  • In this study we developed the analytical methods for the determination of three neurotoxin; anatoxin-a, saxitoxin and neosaxitoxin using HPLC/FLD system and this analytical methods were applied to real sample; algae culture and algae extracts. For the HPLC/FLD analysis of anatoxin-a samples were concentrated on WCX(Weak Cation Exchanger) SPE and then anatoxin-a in concentrate was derivatized with NBD-F solution. Supernatant was injected on HPLC system. For the HPLC/FLD analysis of saxitoxin and neosaxitoxin samples were separated on the column and then derivatizied by post column reactor for fluorescen detection. For post column reaction of saxitoxin we feed two kinds of reaction solution; Oxidizing Reagent of which composition was periodic acid(7mM) in 50mM potassium phosphate buffer, pH 9 and acidifying reagent of which Composition was 0.5M acetic acid. The LOD value for anatoxin-a, saxitoxin and neosaxitoxin in HPLC/FLD method was 24.3 ng. $35{\mu}g/L$, $27{\mu}g/L$ respectively. We determined the anatoxin-a content of lyophilized anabaena flos-aquae and $20{\mu}g/g$ d.w. of anatoxin-a was detected. We analyzed saxitoxin and neosaxitoxin in algae culture media and extracts of lypopyllized algal cell cultured and that of Deachung reservior. Saxitoxin and neosaxitoxin in real sample were below the limit of detection. Although there are various water treatment processes for removing neurotoxins were suggested no process give simultaneous and complete removal of neurotoxins. It was cocluded that nanofiltration which reject material by size can be a process for removal of neurotoxins.

시판 쪽 분말염료의 색소 함량에 따른 면직물의 색상 및 항균성 비교연구 (Analysis of the Pigment Contents of Commercial Indigo Powders and Their Effect on the Color and the Antimicrobial Function of Dyed Cotton Fabrics)

  • 오지은;안춘순
    • 한국의류학회지
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    • 제37권1호
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    • pp.17-26
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    • 2013
  • Market available fermented indigo powders of Indian origin (FI1, FI2), Chinese origin (FC1, FC2), and raw indigo powders of Indian origin (R1, R2) were examined using TLC and HPLC analyses to investigate their pigment contents. TLC analysis gave $R_f$ values of 0.81 and 0.72 for blue and red pigments, respectively. All the powder products and the synthetic and natural indigo standards eluted at 6.9 min and 8.3 min in the HPLC chromatograms, and the peaks showed the ${\lambda}_{max}$ at 610nm and 542nm, representing indigotin and indirubin, respectively. The pigment content calculated based on the area of indigotin and indirubin peaks in the HPLC chromatograms showed that the indigotin content was higher in FC1 and FC2, while FI1 and FI2 had a higher indirubin content. The relative percentage of indirubin was the highest in R2, but the HPLC peak intensity was quite low. Despite the higher indigotin content in FC1 and FC2, cotton dyed with FI1 and FI2 (versus cotton dyed with FC1 and FC2) showed a higher blue (B) hue, the highest K/S values, and the highest antimicrobial effect.

아미노산의 광학이성화 및 GC, GC/MS, HPLC에 의한 광학이성질체의 분리에 관한 연구 (A Study on the Racemization of Amino acids and its Separation with GC, GC/MS and HPLC)

  • 이재성;홍종기;어연우;김택제
    • 분석과학
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    • 제7권1호
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    • pp.41-52
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    • 1994
  • 아미노산 중 alanine, threonine, isoleucine, leucine, aspartic acid, methionine, glutamic acid, tyrosine을 대상으로 열처리, 산처리, UV 광선 조사, 효소(trypsin)의 영향을 살펴보고 6N-HCl, $105^{\circ}C$로 가열했을 때 이성화하는 정도를 측정하였다. 또한 Mass Spectrometer를 이용할 때 각 아미노산의 fragment되는 과정을 조사하여 GC에서 서로 겹칠 때 분석하는 법을 개발하였다. HPLC에서 cyclodextrin bonded phase를 이용해서 dansyl amino acid의 분리를 시도하였다.

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HPLC를 이용한 인삼 진세노사이드의 최적 분석 조건 및 홍삼 제품과 원료삼의 진세노사이드 함량 분석 (Optimal Analytical Conditions for Panax Ginseng Ginsenosides using HPLC and Ginsenosides Content Analysis of Red Ginseng Products and their Raw Materials)

  • 탁근만;손민희;채희정
    • 한국산학기술학회논문지
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    • 제10권2호
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    • pp.418-424
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    • 2009
  • 인삼사포닌인 진세노사이드의 분석조건을 고성능액체크로마토그래피(HPLC)를 이용하여 최적화하였다. Gradient 조건을 변경하여 최적 분석조건을 확립하였고, 같은 조건하에서 인삼원재료와 홍삼 제품 중의 진세노사이드를 분석하였다. 원재료 중에서는 홍삼이 Rg1, Rb1, Rc, Rb2, Rd를 각각 0.29%, 0.82%, 0.33%, 0.32%, 0.11%를 함유하여 가장 높은 진세노사이드 함량을 보였으며, 여러 가지 홍삼제품 중에서는 홍삼엑기스가 가장 높은 함량을 보였다. 인삼 원료와 제품의 종류마다 진세노사이드 함량에 차이를 보였지만 대부분의 원료와 제품에서 Re, Rb1이 그 중 에서도 가장 높은 함량을 보였다.