• 제목/요약/키워드: HPLC(high performance liquid chromatography)

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질량분석기를 단백질 분석에 적용하기 위한 고성능액체크로마토그래피 최적조건 연구 (A study on the optimal HPLC condition for peptides complex analysis using mass spectrometry)

  • 권성원;박철홍
    • 분석과학
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    • 제16권1호
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    • pp.78-81
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    • 2003
  • Peptides separation in high performance liquid chromatography (HPLC) is very important for the analysis of total proteins using mass spectrometry rather than two-dimensional polyacrylamide gel electrophoresis (2D-PAGE). In this study, we investigated the optimal HPLC condition of peptides for the use of mass fingerprinting. As a result of pursuing a combination of solvent additives for HPLC, water and acetonitile containing both 0.1% trifluoroacetic acid and 0.1% acetic acid respectively showed the most efficient resolution and sensitivity.

HPLC에 의한 시호(柴胡) Saponin의 분리 및 정량 (Separation and Determination of Saikosaponins in Bupleuri Radix with HPLC)

  • 한대석;이덕근
    • 생약학회지
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    • 제16권3호
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    • pp.175-179
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    • 1985
  • The optimal condition for the determination of saikosaponin a and d, the major pharmacologically active saponins of the roots of Bupleurum falcatum, was studied with the conversion of these saponins into diene saponins $(saikosaponin\;b_1\;and\;b_2)$. The complete separation and quantitative analysis of these saponins were performed by the method of high performance liquid chromatography using $NH_2$ column. The conversion of saikosaponin a and d into diene saponins under gastric pH was calculated. Thirty-three percent of saikosaponin a was converted to saikosaponin $b_1$ and 63 percent of saikosaponin d was converted to saikosaponin $b_2$.

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Comparison of Extraction Procedures for the Determination of Capsaicinoids in Peppers

  • Jeon, Geonuk;Lee, Jun-Soo
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1515-1518
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    • 2009
  • The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.

Determination of Authentic Chiisanoside in Acanthopanax senticousus by High Performance Liquid Chromatography

  • Lee, Jeong-Min;Kim, Min-Hye;Lee, Sang-Hyun
    • 한국자원식물학회지
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    • 제20권3호
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    • pp.263-266
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    • 2007
  • High performance liquid chromatography (HPLC) was used for the analysis of chiisanoside in each stem and root of Acanthopanax senticosus collected from South Korea, North Korea, China and Russia. A reverse-phase system using a gradient of H$_{2}$O and acetonitrile as the mobile phase was developed and detection was at 210nm. The analysis was successfully carried out within 30 min. Chiisanoside was measured in the stem and root of A. senticosus collected from various countries.

High Performance Liquid Chromatography에 의한 사과주스의 유기산 분석 (Analysis of Organic Acid in Korean Apple Juice by High Performance Liquid Chromatography)

  • 황혜정;김성수;윤광로
    • 한국식품영양과학회지
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    • 제29권2호
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    • pp.181-187
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    • 2000
  • The contents of organic acid in Korean apple juice were analyzed by HPLC using YMC-peak ODS-AQ column and enzymatic assay. Model apple juices were prepared at the laboratory and commercial apple juices were purchased from the market. Individual organic acid contents were as follows: DL-malic acid 62~402mg%, L-malic acid 48~360mg%, citric acid 1.81~15.74mg%, fumaric acid nd~0.50mg%. Together, these tests gave useful information about the quality and authenticity of a particular apple juice smaple. The presence of D-malic acid was a clear indication of adulteration because this isomer did not occur naturally. Fumaric acid and citric acid levels above trace amounts were also inconsistent with pure apple juice.

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아세틸아세톤 유도체화 시약과 HPLC를 이용한 미량 포름알데하이드 수질분석 (Determination of Trace Amounts of Formaldehyde in Water Using High Performance Liquid Chromatography and Acetylacetone as a Derivative Reagent)

  • 이기창;박재형;이원태
    • 대한환경공학회지
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    • 제37권2호
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    • pp.81-86
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    • 2015
  • 수중에 존재하는 포름알데하이드(formaldehyde)를 ${\mu}g/L$ 단위 농도까지 정량할 수 있는 간단한 분석법을 개발하였다. 시료 전처리시 유도체화 시약으로 아세틸아세톤(acetylacetone)을 사용하였고, 기존 분석방법과 달리 추출 및 농축과정을 거치지 않는 것이 장점이다. 시료에 유도체화 시약을 첨가하고 $80^{\circ}C$에서 30분 반응시킨 후 HPLC를 이용하여 포름알데하이드를 분석하였다. 본 방법에 대한 정도보증 결과, 방법검출한계 및 정량한계는 각각 1.6, $5.0{\mu}g/L$로 기존 분석법에 비하여 낮았다. 정밀도 및 정확도는 각각 0.6~3.0%, 91.6~106.3%로 우수하였다. 또한 다양한 환경시료에 대한 회수율 검증에서도 92.0~115.2%로 양호하게 나타났다.

HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법 (Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • 한국동물위생학회지
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    • 제27권1호
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    • pp.17-29
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    • 2004
  • A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

HPLC-DAD를 이용한 갈근탕 중 4종 성분의 동시분석법 확립 (Simultaneous Determination of Four Bioactive Constituents in Galgeun Tang by HPLC/DAD.)

  • 원진배;전원경;마진열;마충제
    • 생약학회지
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    • 제40권3호
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    • pp.224-228
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    • 2009
  • For the quality control of traditional herbal medicine, Galgeun tang, simultaneous determination of glycyrrhizin, paeoniflorin, puerarin, 6-gingerol was established by using a high performance liquid chromatographic (HPLC) method with diode array detector. To separate five four constituents, DIONEX $C_{18}$ column ($5{\mu}m$, $120{\AA}$, $4.6\;mm{\times}150\;mm$) was used with gradient elution system of water and methanol. Validation of the chromatography method was evaluated by linearity, recovery, and precision test. Calibration curve of standard components showed excellent linearity ($R^2$>0.9906). Limits of detection (LOD) and limits of quantification (LOQ) varied from 0.15 to $0.52{\mu}g$/ml and 0.27 to $0.80{\mu}mg$/ml, respectively. The relative standard deviations (RSDs) of data of the intra-day and inter-day experiments were less than 2.88% and 1.21%, respectively. The results of recovery test were ranged from 96.71 to 106.29% with RSD values 0.01-0.80%.

Development of an analytical method for the quantification of oleanonic acid from mastic gum using HPLC/PDA

  • Hak-Dong Lee;Chang-Dae Lee;So Yeon Choi;Sanghyun Lee
    • Journal of Applied Biological Chemistry
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    • 제66권
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    • pp.67-72
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    • 2023
  • A simple and accurate method was developed for the quantitative analysis of oleanonic acid (OA) from mastic gum. The analysis was carried out using reverse-phase high-performance liquid chromatography combined with a photodiode array detector (HPLC/PDA). Our optimized method was validated by measuring various parameters, using an INNO C18 column fitted with a gradient elution system. The results revealed limits of detection and quantification of 0.34 and 1.042 ㎍/mL, respectively. The OA calibration curve exhibited excellent linearity over the concentration range of 0.0625 to 2.0 mg/mL, with r2 =0.9996. Accuracy tests revealed a high recovery rate of 99.44-103.66%, with precision values below 0.15%. These results suggest that the present analytical method can identify and quantify OA in mastic gum with high precision. The HPLC approach developed in this study might be applied to routine analyses and large-scale extraction procedures for OA content quantification.

아연피리치온을 유효성분으로 표기한 화장품류에서 미표기 성분인 베타메타손 유도체의 검출 (Detection of Undeclared Betamethasone Derivatives in Cosmetic Products Labeled to Contain Zinc Pyrithione as the Active Ingredient)

  • 이정표;박성환;양성준;김선미;손경훈;윤미옥;최상숙
    • 대한화장품학회지
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    • 제35권1호
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    • pp.11-17
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    • 2009
  • 스테로이드 함유 표시가 없는 화장품에서 항염증 효과가 있는 글루코코티코스테로이드인 베타메타손프로피오네이트 성분이 검출되었다. 이 화장품은 외용스프레이 및 샴푸로서 주성분으로 아연피리치온을 함유하는 것으로 표기되어 있었다. 화장품에서 스테로이드 구조와 활성을 갖는 물질의 존재를 확인하기 위하여 실리카겔 박층판을 이용한 박층크로마토그래프를 사용하였으며 이 성분을 분리하기 위해 high-performance liquid chromatography (HPLC)를 이용하여 확인 및 정량을 수행하였다. 분취용 HPLC를 이용하여 스테로이드를 함유한 것으로 판단되는 분획을 모은 다음 nuclear magnetic resonance (NMR) 및 mass spectrometry (MS)를 이용하여 스테로이드 성분을 확인하였다. 스테로이드 표준물질로 베타메타손 17-프로피오네이트 및 베타메타손 21-프로피오네이트를 합성하여 사용하였고 이 표준물질과 HPLC 크로마토그램을 비교하여 스테로이드 성분의 함량을 분석하였다. 이 방법으로 아연피리치온 제제와 같은 일부 시판 화장품에서 스테로이드 성분을 확인하였고 reversed-phase high-performance liquid chromatography (RP HPLC) 상의 유지시간 비교를 통하여 스테로이드 성분을 정량한 결과 시험한 총 8종의 화장품 시료 중 2개 제품에서 0.005 ${\sim}$ 0.02%의 베타메타손프로피오네이트가 검출되었다.