• 제목/요약/키워드: HPLC detector

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Development of Analytical Methods for Insect Moulting Hormone $({\beta}-Ecdysone)$ by HPLC/UV Using Boronate Derivatization

  • Shim, Jae-Han;Kim, In-Seon;Lim, Kye-Taek
    • Applied Biological Chemistry
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    • v.41 no.4
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    • pp.251-256
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    • 1998
  • The analytical method of ${\beta}-ecdysone$, the insect moulting hormone, by high performance liquid chromatograph (HPLC) with UV detector was developed using boronic ester derivatization and applied to the extracts of Ajuga iva, Silene otites and Schistocerca egg. Derivatization of yield with methyl-, butyl-, and phenyl-boronate was completed under mild conditions with 20-hydroxyecdysone. The conversion ratios of boronate were estimated to be 70% in methylboronic acid, 89% in butylboronic acid and 93% in phenylboronic acid. Phenylboronate showed a high sensitivity and demonstrated an effective separation on HPLC. The optimum temperature and reaction time for derivative formation were $25^{\circ}C$ and 20 min. respectively. ${\beta}-Ecdysone$ was effectively identified in extracts of Ajuga iva, Silene otites and Schistocerca egg by the HPLC method.

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Microanalysis of Metocurine Iodide in Urine and Blood by HPLC (HPLC를 이용한 뇨 및 혈액중 Metocurine Iodide의 미량분석)

  • Kim, Kyung-Nim;Lee, Jong-Pil;Kim, Hyo-Jin;Kim, Bak-Kwang
    • YAKHAK HOEJI
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    • v.38 no.4
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    • pp.379-388
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    • 1994
  • A new method for the analysis of metocurine iodide in biological fluids was developed. Metocurine iodide was quantitatively extracted with rose bengal from aqueous layer into dichloromethane layer and the amount of metocurine iodide was calculated from the amount of rose bengal which was determined by HPLC with fluorescence detector. It was possible to analyze metocurine iodide without the effect of co-prescribed drugs in the concentration range of $0.09{\sim}9.10\;{\mu}g/ml$. The detection limits of metocurine iodide in urine and blood were 0.8 and 1.2 ng at S/N=3, each respectively.

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Compositional Sugar Analysis of Antitumor Polysaccharidees by High Performance Liquid Chromatography and Gas Chromatography

  • Kim, Yeong-Shik;Park, Kyung-Shin;Park, Ho-Koon;Kim, Sung-Whan
    • Archives of Pharmacal Research
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    • v.17 no.5
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    • pp.337-342
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    • 1994
  • Carbohydrate analysis is important in studying structure and activity of complex polysaccharides. New analytical method was applied to get an information on the composition of polysaccharides showing antitumor activity. Monosaccharides were labeled with 7-amino-1, 3-naph-thalenedisulfonic acid (7-AGA) by reductive amination and separated by HPLC. Five kinds of polysaccharides from Basidiomycetes were hydrolyzed and analyzed in combination with electrophresis and HPLC. At the same time, alditol acetate derivatives were prepared and analyzed by gas chromatography. Two different techniques using different derivatization methods showed very similar results. The monosaccharides from Coriolus versicolor and Cordyceps militaris were glucose and galactose. Phellinus linteus composed of glucose, glactose, mannose, arabinose and fucose. The HPLC method with fluorescence detector was very sensitive compared to other methods.

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Simultaneous determination of bisphenol A, chlorophenols and alkylphenols by solid-phase extraction and HPLC

  • Lee, Taejoon;Park, Keun-Young;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.30 no.1
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    • pp.20-25
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    • 2017
  • An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

The Simultaneous Analysis of Oxytetracycline, Chloramphenicol and Sulfamethoxazole in Pork by HPLC (HPLC를 이용한 돈육 중의 Oxytetracycline, Chloramphenicol 및 Sulfamethoxazole의 동시검출)

  • 조혜연;조진국;이치호
    • Food Science of Animal Resources
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    • v.21 no.1
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    • pp.64-70
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    • 2001
  • The extraction procedure and HPLC condition were modified to analyze the residues of oxytetracycline, sulfamethoxazole and chloramphenicol in pork, simultaneously. The antibacterial agents in pork were extracted with 0.02M EDTA-Mcilivine buffer:ethanol:acetonitrile (5:3:2). After the removal of fat with n-hexane, the extracts were evaporated and purified with Sep-pak $C_{18}$ cartridge column using 0.01M oxalic acid 0.1% (v/v) triethylamine (TEA) in acetonitrile. The peak of antibacterial agents was detected with $\mu$ Bondapak C18 column, UV detector (280nm) and 0.01M oxalic acid: methanol: acetonitrile (7.5:2.0:0.5). Detection limits for three antibacterial standards were 0.03 ppm. Calibration curves were linear between 0.03 and 2.0 ppm (R$^2$>0.999). When spiked the level of 1.0 ppm of oxytetracycline, sulfamethoxazole and chloramphenicol into meats, the recoveries from meats were 77.3%, 79.7% and 59.3%, respectively. These results showed that the modified extraction method provided good analytical resolution and the recoveries of the above antibacterial agents in meats.

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Studies on the Content of Pueraria Radix in the Tea by HPLC (HPLC에 의한 한국산 칡차의 분석)

  • 김명희;박성배
    • Journal of Food Hygiene and Safety
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    • v.2 no.3
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    • pp.89-95
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    • 1987
  • This studies was performed to investigate the quality control of Pueraria RadiI tea. Experimental subjects were 8 kinds of tea and wet and dry Pueraria RadiI which were collected from the Seoul area. For standards, Daidzein and Daidzin were isolated from Pueraria Radix. Analysis method was carried out by HPLC using ${\mu}-Bondapark{\;}C_{18}$ column and UV 254 nm detector. Samples were extracted with methanol by Cold method (at room temperature for 24 hours) and Hot extraction method (at $^{\circ}C$ for 4 hours) Pueraria radix contained 0.08% Daidzein and 0.66% Daidzin Most of the Pueraria Radix tea contained extract of Pueraria Radix less than the labled amounts listed.

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Determination and Ethylene Oxide(EO) Separation of Polysorbates by RP-HPLC (역상 HPLC에 의한 polysorbates의 산화에틸렌(EO) 분리 및 정량분석)

  • Lee, Yong-Hwa
    • Journal of the Korean Applied Science and Technology
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    • v.29 no.4
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    • pp.585-593
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    • 2012
  • The EO separation and quantitative determination of polysorbate 20, polysorbate 40, polysorbate 60 and polysorbate 80 was carried out by reversed phase HPLC. The water/acetonitrile was used for the mobile phase of gradient conditions. An YMC Pack Ph ($250mm{\times}4.6mm$ i.d., $5{\mu}m$) and Phenomenex C4 ($250mm{\times}4.6mm$ i.d., $5{\mu}m$) and the selected ELSD detector was applied. The analysis results of HPLC showed good linearity with correlation coefficient of $r^2$=0.997 in the rage of $180.2{\sim}980.5{\mu}g/mL$ and detection limit.

Determination of thyroid hormones in plasma samples by high performance liquid chromatograph/diode array detector/electrospray ionization mass spectrometer (HPLC/DAD/ESI-MS를 이용한 혈장시료 중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.424-433
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    • 2007
  • An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

Analytical Optimum of Ginsenosides according to the Gradient Elution of Mobile Phase in High Performance Liquid Chromatography (HPLC의 이동상 용매조건에 따른 인삼 Ginsenoside 분석)

  • Park, Ji-Yeong;Won, Jun-Yeon;Lee, Chung-Yeol
    • Korean Journal of Medicinal Crop Science
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    • v.15 no.3
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    • pp.215-219
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    • 2007
  • This study was conducted to analyze not only for the quality guaranteed of red ginseng but also for the minor ginsenosides. Although several studies have reported to analyze ginseng saponins, those were focused to major saponins, including 6 to 7 ginsenosides. As increase of interest in medicinal effect of ginseng products, anasis of various ginsenosides in both red and white ginseng are strongly demanded. To perform optital condition of 12 ginsenoside analysis, We controlled HPLC conditions, such as the gradient elution of the mobile phase. We found the adequate separation method for 12 ginse-nosides. The optimum condition was as following : H$_2$O/CH$_3$CN ratios were 82/18, 70/30, 55/45 and 50/50, respectively. Sol-vent flow rate was 1.00 ma/min. Column temperature was kept to 35$^{\circ}$C. UV detector was set to 203 nm.

Simultaneous Analysis of Six Compounds in Yijin-tang by HPLC-PDA (HPLC-PDA을 이용한 이진탕 중 6종 성분의 동시분석)

  • Kim, Seong-Sil;Kim, Jung-Hoon;Shin, Hyeun-Kyoo;Seo, Chang-Seob
    • Herbal Formula Science
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    • v.21 no.1
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    • pp.71-79
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    • 2013
  • Objectives : Yijin-tang has been used in the treatment of gastrointestinal diseases such as irritable bowel syndrome, gastritis, and gastric ulcer. In this study, a high-performance liquid chromatography (HPLC) method was established for simultaneous analysis of six compounds, liquiritin, glycyrrhizin, hesperidin, 6-gingerol, homogentisic acid, and 3,4-dihydroxybenzaldehyde in Yijin-tang, a traditional Korean herbal medicinal preparation. Methods : A Gemini C18 column was used for the separation of six constituents at $40^{\circ}C$. The mobile phase using gradient elution consist of two solvent systems, 1.0% acetic acid in water (A) and 1.0% acetic acid in acetonitrile (B). The flow-rate was 1.0 mL/min and injection volume was $10{\mu}g$. The detector was a photodiode array (PDA) detector set at 254 nm and 280 nm. Results : The calibration curves of six compounds showed good linearity in various concentration ranges ($R^2{\geq}0.9997$). The limits of detection (LOD) and limits of quantification (LOQ) were 0.028-$0.192{\mu}g/mL$ and 0.093-$0.540{\mu}g/mL$, respectively. The RSD (%) of the intra and inter day validations were 0.03-0.84% and 0.05 -1.00%, respectively. Recovery was 96.14-01.90% and RSD (%) was less than 1.5%. Conclusions : The established simultaneous analysis methods will help management to improve the quality of Yijin-tang.