• 제목/요약/키워드: high performance liquid chromatography

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고속액체 크로마토크래피에 의한 커피, 홍차, 녹차중의 카페인 정량에 관한 연구 (A Study on the Determination of Caffeine in Coffee, Black tea and Green Tea by high performance Liquid Chromatography)

  • 권익부;이윤수;우상규;이충영;서준걸
    • 한국식품위생안전성학회지
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    • 제5권4호
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    • pp.213-217
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    • 1990
  • 커피, 홍차, 녹차중의 카페인 함량을 간단하고 신속하게 정량하는 방법을 검토하였다. 역상계 액체크로마토그래피에 의한 카페인 정량은 메타놀-초산-물(20 : 1 : 79)을 이동상으로 하여 ${\mu}-Bondapak$ C18 컬럼하에서 이루어졌다. 카페인의 검출에는 UV검출기를 사용하여 280 mm에서 행하였다. Sep-Pak alumina A 카트리지를 이용한 간단한 전처리를 통해 효과적으로 카페인의 추출 및 clean-up를 행하였다. 카페인의 첨가 회수율은 95.2~101.3%이었고 분석의 재현성은 상대표준 편차로서 0.10~0.62%이었으며 검출한계는 $0.1;\mu\textrm{g}$/ml이었다.

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고성능 액체크로마토그래피를 이용한 식이보충제에서 크레아틴, 디시안디아마이드, 디하이드로트리아진의 동시분석 (Simultaneous Determination of Creatine, Dicyandiamide and Dihydrotriazine in Dietary Supplements by High Performance Liquid Chromatography)

  • 박상욱;유명상;이원재
    • KSBB Journal
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    • 제29권4호
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    • pp.232-238
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    • 2014
  • The simultaneous determination of creatine monohydrate (CrM), dicyandiamide and dihydrotriazine in dietary supplements using reversed-phase high performance liquid chromatography (HPLC) was developed. Chromatography was performed on a Nuclosil 100-5 SA ($4.6{\times}250mm$) column with a mobile phase of 2.3% ammonium phosphate (pH 5.5), and UV detection at 224 nm, 212 nm, and 237 nm, respectively. The performance characteristics of HPLC were determined in terms of selectivity, linearity, precision, recovery, limit of detection (LOD), and limit of quantification (LOQ). The calibration curves were linear within the concentration range of $40.0{\sim}500.0{\mu}g/mL$ for creatine, $0.1{\sim}12.8{\mu}g/mL$ for dicyandiamide, and $0.05{\sim}6.4{\mu}g/mL$ for dihydrotriazine. The detection limits of the method were 1.09, 0.01, and $0.08{\mu}g/mL$ for creatine, dicyandiamide, and dihydrotriazine, respectively. The recoveries of creatine, dicyandiamide, and dihydrotriazine were 97.2~100.9, 92.3~106.5, and 97.2~105.5%, respectively. It is expected that the chromatographic analytical method developed in this study will be usefully applicable to simultaneous determination of creatine, dicyandiamide, and dihydrotriazine contained in dietary supplements.

Simultaneous Determination of Sulfonamides in Porcine and Chicken Muscle Using High Performance Liquid Chromatography with Ultraviolet Detector

  • Shim, You-Sin;Shin, Dong-Bin;Cho, Yong-Sun;Choi, Yun-Hee;Lee, Sang-Hee
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1430-1434
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    • 2009
  • The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of $50-150\;{\mu}g/kg$ was obtained with the correlation coefficient ($r^2$) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and $7-96\;{\mu}g/kg$ in porcine muscle, and 4-32 and $13-97\;{\mu}g/kg$ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than $100\;{\mu}g/kg$.

Rapid Isolation of Cyanidin 3-Glucoside and Peonidin 3-Glucoside from Black Rice (Oryza sativa) Using High-Performance Countercurrent Chromatography and Reversed-Phase Column Chromatography

  • Jeon, Heejin;Choi, Janggyoo;Choi, Soo-Jung;Lee, Chang Uk;Yoon, Shin Hee;Kim, Jinwoong;Yoon, Kee Dong
    • Natural Product Sciences
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    • 제21권1호
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    • pp.30-33
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    • 2015
  • Anthocyanins are water soluble plant pigments which are responsible for the blue, red, pink, violet colors in several plant organs such as flowers, fruits, leaves and roots. In recent years, anthocyanin-rich foods have been favored as dietary supplements and health care products due to diverse biological activities of anthocyanins including antioxidant, anti-allergic, anti-diabetic, anti-microbial, anti-cancer and preventing cardiovascular disease. High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase medium pressure liquid chromatography (RP MPLC) method was applied for the rapid and efficient isolation of cyanidin 3-glucoside (C3G) and peonidin 3-glucoside (P3G) from black rice (Oryza sativa L., Poaceae). The crude black rice extract (500 mg) was subjected to HPCCC using two-phase solvent system composed of tert-butyl methyl ether/n-butanol/ acetonitrile/0.01% trifluoroacetic acid (TBME/B/A/0.01% TFA, 1 : 3 : 1 : 5, v/v, flow rate - 4.5 mL/min, reversed phase mode) to give enriched anthocyanin extract (37.4 mg), and enriched anthocyanin extract was sequentially chromatographed on RP-MPLC to yield C3G (16.5 mg) and P3G (8.7 mg). The recovery rate and purity of isolated C3G were 76.0% and 98.2%, respectively, and those of P3G were 58.3% and 96.3%, respectively. The present study indicates that HPCCC coupled with RP-MPLC method is more rapid and efficient than multi-step conventional column chromatography for the separation of anthocyanins.

High performance liquid chromatography를 이용한 빈카민 분석 및 빈카마이너의 항산화능 측정 (Analysis of Vicamine Using High Performance Liquid Chromatography and Antioxidant Activity of Vincaminor Extract)

  • 정종희;백유미;이광근
    • 한국식품과학회지
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    • 제40권5호
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    • pp.599-602
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    • 2008
  • 빈카마이너 유효 성분인 빈카민은 인돌알카로이드의 일종으로 뇌혈관 질환 치료에 자주 사용 되어 왔다. 빈카마이너의 항산화능을 알아보기 위하여, 빈카마이너 추출액과 빈카민의 항산화능을 DPPH와 lipid MA 측정법으로 측정하였다. 빈카마이너 잎을 분쇄하여 물, 메탄올, 에탄올 용매로 추출하였다. 추출물의 항산화능은 추출용매와 측정방법에 따라 상이한 결과를 보였다. DPPH 방법으로 항산화능을 측정한 결과, 물 추출액에서 가장 높은 항산화능을 보였다. 그러나 lipid MA 측정법에 의한 결과에서는 에탄올 추출액이 5,000 ${\mu}g/mL$ 농도에서 대구 간유의 MA 형성을 82%까지 저해시킨 것으로 나타나 가장 높은 항산화능을 보였다. 빈카마이너 추출액 중 빈카민은 HPLC에 의해 분석되었으며 빈카민의 함량은 0.42$\pm$0.005 ${\mu}g/mL$이었다.

Marker compounds contents of Salvia miltiorrhiza Radix depending on the cultivation regions

  • Seong, Gi-Un;Kim, Mi-Yeon;Chung, Shin-Kyo
    • Journal of Applied Biological Chemistry
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    • 제62권2호
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    • pp.129-135
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    • 2019
  • Salvia miltiorrhiza Radix is cultivated in Korea and China and is traditionally used to treat cardiovascular diseases. In this study, we developed and validated a quantitative analysis method for S. miltiorrhiza Radix using high-performance liquid chromatography (HPLC). Identification was performed using ultra performance liquid chromatography-tandem mass spectrometry. For quantitative analysis, we used seven marker compounds. Separation conditions for HPLC were optimized using an ODS column with gradient conditions of 1% formic acid in distilled water and 1% formic acid in acetonitrile, with a flow rate of 0.8 mL/min and a detection wavelength of 280 nm. This method showed good linearity ($R^2=0.9998$), precision (relative standard deviation ${\leq}3.3%$), accuracy (recovery of 94.16-102.89%), limit of detection ($7.53{\mu}g/mL$), and limit of quantification ($23.71{\mu}g/mL$). This approach successfully quantified marker compounds in S. miltiorrhiza Radix. The individual marker compounds were identified by comparing the molecular masses and retention times with does standard compounds. Marker compound contents of S. miltiorrhiza Radix were investigated with different cultivation regions. Seven marker compounds were detected and quantified in all samples. Among them, salvianolic acid B showed the highest contents and it ranged from 4.13 to 7.15%. The salvianolic acid B content (7.15%) of marker compound was the highest in Bonghwa, and the tanshinone IIA content (1.90%) was the highest in Pohang. The results of marker compounds and developed method were intended to provide a favorable reference for the study of S. miltiorrhiza Radix from different regions of Korea.

한약처방의 표준화를 위한 HPTLC의 활용 (The Application of High Performance Thin Layer Chromatography for Herbal Formula Standardization)

  • 최민경;김형극;왕경화;손창규
    • 대한한의학회지
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    • 제32권4호
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    • pp.68-74
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    • 2011
  • Objective: The purpose of this study is to expatiate on high performance thin layer chromatography (HPTLC) as a simple, easy and scientific method for evaluation and standardization of herbal formulae. Methods: Through retrieving HPTLC application for herbal formulae in the literatures, the current situation of HPTLC application, and potential as well as limitation of HPTLC as a standardization method for multi-herbal drug was studied. Results: HPTLC is a speedy, inexpensive and well-operable tool for possessing multi-capability on component identification, separation, quantification and purification compared to other methods, such as high performance liquid chromatography (HPLC), gas chromatography (GC). Conclusions: HPTLC is considered as an available and convenient method for quality control and standardization of multi-herbal drugs. Thereby, this method could be recommended to widely applicate in the traditional Korean medicine.

HPLC-MSD 를 이용한 식육 중 합성항균제의 동시분석 (Simultaneous detection for synthetic antimicrobials in muscle by high performance liquid chromatography-mass selective detector (HPLC-MSD))

  • 홍인석;최윤화;권택부;이정학
    • 한국동물위생학회지
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    • 제29권3호
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    • pp.317-330
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    • 2006
  • This study was conducted to develop the analytical method about simultaneous determination for synthetic antimicrobials in muscle by high performance liquid chromatography - mass selective detector (HPLC- MSD). Solid phase extraction (SPE), matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) have been adapted as pretreatment procedures for HPLC- MSD. Among various solvent tested, methanol was chosen for extraction of synthetic antimicrobials in muscles. For the optimized response, the values of various MS parameters including fragment voltage, drying gas flow, nebulizer pressure, drying gas temperature were verified. The average recovery rates using MSPD and SPE for muscles of bovine and pork were 78.9-127.1% and 78.3-121.7%, respectively. This method was verified the satisfactory performance for fourteen synthetic antimicrobials excepting carbadox in muscle of pork as detection limit of $0.05{\mu}g/g$ on API/ES SIM mode.

황금(Scutellaria baicalensis) 유효분획물 제조의 합리적이고 효율적인 접근방법 (Rational and efficient approach to the preparation of the active fractions of Scutellaria baicalensis)

  • 김두영;김원준;김정희;오세량;류형원
    • Journal of Applied Biological Chemistry
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    • 제62권1호
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    • pp.31-38
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    • 2019
  • Scutellaria baicalensis Georgi (Scutellariae Radix)는 이뇨제, 고지혈증, 항박테리아, 항알레르기, 항염증제 및 항암제와 같은 건강보조식 및 전통 생약으로도 널리 사용되어 왔다. 본 연구에서 복잡한 S. baicalensis 추출물에서 지표 물질 또는 유효화합물들을 분리하는 것은 신원 확인 및 생리활성 평가를 위한 필수적인 단계다. 8개의 성분들로 구성된 타겟 분획물을 두개의 gradient elution를 사용하여 고성능 액체 크로마토 그래피에서 분석하였다. 중압 액체크로마토그래피 및 개방형칼럼으로 분취를 시뮬레이션함으로 예비실험에서 충분히 분리가 되도록 용리 조건을 결정할 수 있었다. 최적 분취방법으로 확보된 표준유효분획물로부터 8개의 지표성분들이 포함된 것을 확인하였다. 또한, 분획물은 UPLC-QTof-MS 비교 분석으로 MS, UV, HRESIMS 결과를 확인할 수 있었다. 따라서, 스케일 업 실험법은 S. baicalensis 추출물에 성공적으로 적용될 수 있었다.