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

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액체크로마토그래피를 이용한 벌꿀 중 테트라싸이클린계 항생물질의 정량분석 및 잔류조사 (Determination and survey of tetracyclines residue in honey by high performance liquid chromatography)

  • 이성모;박은정;홍지영;김정임;이정구;황현순;김용희
    • 한국동물위생학회지
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    • 제28권3호
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    • pp.203-213
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    • 2005
  • Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

Metabolite Analysis of Panax ginseng C. A. Meyer by HPLC According to Root Age

  • Shin, Yoo-Su;Lee, Min-Jeong;Bang, Kyong-Hwan;Kim, Seon-Young;Lee, Sung-Sik;Hyun, Dong-Yoon;An, Tae-Jin;Cha, Seon-Woo;Seong, Nak-Sul
    • Food Science and Biotechnology
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    • 제16권4호
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    • pp.636-640
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    • 2007
  • In order to investigate the major metabolite patterns of aged Panax ginseng C.A. Meyer roots, the ginsenoside contents for white ginseng roots of various ages were compared. The 1-year to 6-year old roots were extracted with methanol, and then the methanol-soluble metabolites were analyzed by high performance liquid chromatography (HPLC). The metabolite contents of the 1-year and 2-year roots, including the ginsenosides and minor components, were not different, but the $Rg_1$, Re, and Rc ginsenoside contents between the 2-year and 3-year roots showed significant differences. $Rg_1$ and Rc increased significantly in the 1-year to 2-year roots, and Re increased significantly from the 3-year root age. Rd increased slightly until the 2-year age and decreased from the 3-year age. Based on the ginsenoside distributions and contents at various root ages, we have suggested 2 biogenesis schemes using the ginsenosides that have been isolated from the roots of P. ginseng so far.

Estimation for warfarin in pharmaceutical preparation using monolithic column

  • Zahraa Hadi Shareef;Ahmed Ali Alkarimi
    • 분석과학
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    • 제37권4호
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    • pp.220-229
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    • 2024
  • This study aims to developing a method for estimating pharmaceutical compounds within a monolith column using high-performance liquid chromatography (HPLC). The monolithic column was prepared using copolymerization of glycidyl methacrylate, co-ethylene dimethacrylate, and co-acrylic acid inside a borosilicate tube of specific dimensions a 60 mm borosilicate tube length with 1.5 mm and 3.5 mm inner and outer diameters, respectively. A UV Ultra violet source with a wavelength of 365 nm was used, and the polymerization process involved mixing glycidyl methacrylate, acrylic acid, ethylene dimethacrylate as a binder, and 2,2-dimethoxy-2-phenyl acetate phenone as an initiator in suitable solvents consisting of ethanol and 1-hexanol. The polymerization process formed the monolith column after 4 minutes, and subsequently, the epoxy groups were altered to diol groups using 0.2 M hydrochloric acid HCl, which were pumped through the column for 3 hours at a flow rate of 10 µL·min-1. Various techniques, such as Scanning Electron Microscope SEM, Brunauer-Emmett-Teller BET, Fourier-transform infrared spectroscopy FT-IR and HNMR, were utilized to characterize and confirm the structure of the monolith. The prepared monolith was employed to estimate and identify the pharmaceutical compound of warfarin using high-performance liquid chromatography HPLC. The analytical curve of warfarin was linear in the range of 3 to 100 ㎍·mL-1 with an r2 value of 0.999. The detection and quantification limits were 0.932 and 2.788 ㎍·mL-1, respectively. The molar absorptivity and Sandells sensitivity were 2.99138 × 106 L·mol-1·cm-1 and 103.1 × 10-3 ㎍·cm-2, respectively.

인간 항균펩타이드인 LL-37 유래의 FK-13의 화장품보존제로 활용에 대한 연구 (A Study on the Use of Human Antibacterial Peptide LL-37-derived FK-13 as a Cosmetic Preservative)

  • 윤효숙;최용준;양재찬;민혜정
    • 한국응용과학기술학회지
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    • 제38권6호
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    • pp.1568-1576
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    • 2021
  • 본 연구에서는 인체에 보다 안전한 천연 화장품보존제 발굴을 목표로 하여 인간유래 항균펩타이드 LL-37의 짧은 유사체인 FK-13을 화장품보존제로 사용하고자 연구를 진행하였다. 이를 위해 13개의 아미노산으로 구성된 FK-13 펩타이드를 고상 펩타이드 합성법로 합성하였고 reversed phase-high performance liquid chromatography (RP-HPLC)로 정제 후 liquid chromatography-mass spectrometry (LC-MS)를 이용하여 순도와 분자량을 확인하였다. 합성된 FK-13을 이용하여 미생물에 대한 방부력을 검정하였고 화장품에 적용 가능성을 살펴보았다. FK-13은 3개의 그람-양성균 (Staphylococcus aureus, Bacillus subtilis, Staphylococcus epidermidis)과 3개의 그람-음성균 (Escherichia coli, Salmonella typhimurium, Pseudomonas aeruginosa), 그리고 진균인 Candida glabrata 에서도 높은 항균 활성을 보였으며 넓은 항균활성 스펙트럼을 나타내었다. 이를 바탕으로 화장품보존제로서의 적합성을 확인하였다. 또한 FK-13은 고온에서 분자의 열안정성을 보였으며 기존의 천연 한방화장품 방부제 및 화학보존제들과의 항균활성 비교 실험에서도 보다 월등한 항균활성 효능을 나타내었다. 따라서 FK-13 펩타이드는 인체 친화적이고 효과적인 항균활성을 나타내므로, 기존 화학보존제를 대체할 새로운 천연 화장품보존제로 적용이 가능할 것으로 판단된다.

HPLC-UV검출방법으로 유도체화를 통한 비테인과 콜린의 동시분석 (Simultaneous determination of betaine and choline using derivatization by HPLC with UV detection)

  • 이인숙;팽기정
    • 분석과학
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    • 제28권2호
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    • pp.112-116
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    • 2015
  • Extraction of quaternary ammonium compounds (choline and betaine) from plant samples (spinach) using ion exchange resin (AG1, OH form) is a very simple and inexpensive approach. However, it is very hard to determine amounts of choline and betaine simultaneously using high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Unlike choline, betaine has low molar absorptivity in UV-visible (UV-Vis) region, which makes it difficult to carry out UV-Vis detection of betaine. The mixture of quaternary ammonium compounds (choline and betaine) was derivatized using 2-bromo acetophenone as a derivatizing agent. As a result, choline did not react with the derivatizing agent, whereas betaine formed a betaine derivative. This betaine derivative exhibited detectable UV absorption with baseline separation between choline and the betaine derivative. Thus, with this method, choline and betaine can be determined simultaneously by using the HPLCUV method through one-step derivatization, which is an easy, sensitive, and reliable method.

HPLC Analysis of Methylated Amino Acids : Methylated Amino Acids on HPLC

  • Park, Kwang-Sook;Hong, Sung-Youl;Lee, Hyang-Woo;Kim, Snag-Duk;Paik, Woon-Ki
    • Archives of Pharmacal Research
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    • 제9권1호
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    • pp.15-18
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    • 1986
  • Various naturally occuring methylated amino acid derivatives were resolved on high performance liquid chromatography (HPLC), using o-phthadialdehyde as a fluorogenic reagent. We separated .$\varepsilon$-N-monomethyllysine, $\varepsilon$-N- dimethyllysine, and $\varepsilon$-N-acetyllysine from lysine derivatives. $N^{G}$-Monomethylarginine and $N^{G}$-dimethylarginine were separated from arginine derivatives. However, $\varepsilon$-N-monomethyllsine and $\varepsilon$-N-trimethyllysine, $N^{G}$, $N^{G}$-dimethylarginine and $N^{G}$, $N^{G}$-dimethylarginine were not resolved under the conditions employed. S-Methylmethionine, S-methylcysteine, and 1-N-methylhistidine or 3-N-methylhistidine were clearly separated from their reference amino acids, even though 1-N-methyl-and 3-N-methylhistidine coul not be separated.

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HPLC 및 신속검출방법을 이용한 우유내 Sulfamethazine의 분석에 관한 연구 (Determination of Sulfamethazine Using High Performance Liquid Chromatography and Several Screening Methods)

  • 김철현;백승천;문지웅
    • 한국식품위생안전성학회지
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    • 제12권1호
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    • pp.71-77
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    • 1997
  • Sulfonamides, a therapeutically important group of antimicrobial drugs, are widely used to treat and prevent the acute systemic and skin infections in dairy cattle. They also pose an economic hazard through inhibition of growth of dairy starter cultures. This study was carried out to compare four screening methods for detection of sulfamethazine in milk and determine the positive milk sample by HPLC method. Sulfamethazine was used to spike at five levels of sulfamethazine. The Lac-Tek test and CharmII test were also consistent better than TTCII test and Delvo SP test in sulfamethazine detection. Analysis probabilities of obtaining a positive response with TTCII test and Delvo SP test assay at 50 ppb sulfamethazine level in milk samples were only 14%, 42% each. Whereas using the Lac-Tek test and CharmII test would have resulted in 100% identification of the five levels. Determination of sufamethazine using the HPLC method in the spiked milk were 10.64, 19.30, 30.76,38.83 and 50.23 ppb, respectively.

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HPLC법에 의한 뇨 중의 Putrescine, Spermidine 및 Spermine의 정량 (Determination of Putrescine, Spermidine and Spermine in urine by HPLC)

  • 신태용;이석봉;김형민
    • 분석과학
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    • 제10권6호
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    • pp.445-452
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    • 1997
  • 뇨 중에 Putrescine, Spermidine 및 Spermine benzoyl chloride를 유도체화제로 처리한 다음 HPLC법으로 정량하였다. ${\mu}$-Bondapak $C_{18}$ 컬럼과 methanol/$H_2O$(50/50v/v)를 사용하여 정상인 및 자궁암 환자의 뇨 중에서 Putrescine, Spermidine 및 Spermine을 역상법으로 분석한 결과 암환자의 경우 정상인에 비해 이들 polyamine이 현저한 증가를 보였다.

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자근의 성분 분리 및 이들 성분의 HPLC-UV 동시분석법 개발 (Isolation of Constituents of Lihtospermum erythrorhizon and Development of an Analytical Method of its Constituents by HPLC-UV)

  • 홍은영;경민지;황완균
    • 약학회지
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    • 제59권5호
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    • pp.222-229
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    • 2015
  • Lithospermi radix, the dried roots of Litospermum erythrorhizon Sieboid et Zuccarini (Boraginaceae), has long been used to treat detoxification and inflammation. In this study, we isolated two main quinoid compounds, ${\beta}$-hydroxyisovalerylshikonin (1) and acetylshikonin (2) from L. erythrorhizon. As acetylshikonin is considered as a marker compound of L. erythrorhizon, a rapid analysis method for the simultaneous determination of quinoid compounds including 2 was also developed by HPLC (High Performance Liquid Chromatography) and validation of this analytical method. By the developed method, two quinoid marker compounds (${\beta}$-hydroxyisovalerylshikonin and acetylshikonin) were successfully quantified in 31 commercial samples which were collected from different regions. The contents were 0.20% (${\beta}$-hydroxyisovalerylshikonin) and 0.22% (acetylshikonin), respectively.

Extraction and separation of glabridin from licorice by reversed phase high performance liquid chromatography

  • Choi, Du Young;Row, Kyung Ho
    • 분석과학
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    • 제19권6호
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    • pp.455-459
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    • 2006
  • The extraction and separation of glabridin from licorice root by HPLC was performed in this work. First, by investigating the different extraction solvents, extraction methods and extraction times, a one-hour ultrasonic extraction procedure with ethyl acetate as the extraction solvent was optimized. Then the ethyl acetate extraction was applied to RP-HPLC for separation of glabridin. The column efficiencies and resolutions were experimentally investigated with different mobile phase compositions. Baseline separation of glabridin was obtained under the mobile phase composition of 50/50 vol.% (ACN/water). The retention time of glabridin was 20.3 min. The peak of glabridin was collected from the HPLC elution for several times and identified by LC/MS. Under the optimum extraction and HPLC separation methods, 1.26 g of glabridin per kg licorice root could be extracted.