• Title/Summary/Keyword: High-performance liquid chromatography analysis

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Determination of Monocrotophos Residues by HPLC

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.245-250
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    • 2004
  • An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

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

  • Kwon, Sung Won;Park, Chul Hong
    • Analytical Science and Technology
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    • v.16 no.1
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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.

Separation of Tetrodotoxin, DHA and EPA from Pufferfish Liver Waste (복어간 폐기물로부터 Tetrodotoxin, DHA 및 EPA의 분리)

  • 차병윤;최진석;임정규;이동익;이원갑;이은열;김희숙;김동수
    • Journal of Life Science
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    • v.10 no.2
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    • pp.115-124
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    • 2000
  • The present study was undertaken to separate the available components effectively, such as tetrodotoxin(TTX), docosahexaenoic acid(DHA, C22:6,ω-3) and eicosapentaenoic acid (EPA, C20:5,ω -3) from pufferfish liver waste, which are known to have high values as bioactive materials. By using ultrafiltration, it was possible to separate high contents of 68mg TTX from pufferfish liver waste. In contrast, by activated charcoal column, it was to obtain about 54mg TTX. The recovering ratios were 65.3% and 45.0% in the two different methods of ultrafiltration and activated charcoal column, respectively. From the results of HPLC and gas chromatography-mass spectrometry(GC-MS), the obtained toxins were identified to be TTX and its derivatives. In addition, it was also possible to obtain 72.3g DHA and 11.4g EPA from 1kg of pufferfish liver by high performance liquid chromatography (HPLC). These amounts of DHA and EPA were also 17.70% and 1.04% in the total lipid of pufferfish liver oil from analysis of gas chromatography(GC), respectively.

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Octadecyl-Modified Graphene as an Adsorbent for Hollow Fiber Liquid Phase Microextraction of Chlorophenols from Honey

  • Sun, Meng;Cui, Penglei;Ji, Shujing;Tang, Ranxiao;Wu, Qiuhua;Wang, Chun;Wang, Zhi
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1011-1015
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    • 2014
  • Octadecyl-modified graphene (graphene-C18) was fabricated and used as adsorbent in hollow fiber liquid phase microextraction (HF-LPME) for the first time. The extraction performance of graphene-C18 reinforced HF-LPME was evaluated using chlorophenols as model analytes. The factors affecting the extraction efficiency, such as extraction time, pH of the sample solution, agitation rate, the concentration of graphene-C18 and salt addition were optimized. After the graphene-C18 reinforced HF-LPME of the chlorophenols from honey sample, the analytes were separated and determined by high-performance liquid chromatography. The linearity was observed in the range of 5.0-200.0 ng $g^{-1}$ for 2-chlorophenol and 3-chlorophenol, and 2.0-200.0 ng $g^{-1}$ for 2,3-dichlorophenol and 3,4-dichlorophenol, respectively. The limits of detection (S/N = 3) of the method were lower than 1.5 ng $g^{-1}$. The recoveries of the method were between 88% and 108%. The method is simple, sensitive and has been resoundingly applied to analysis of chlorophenols in honey samples.

Antioxidant Activity of Fractions from 70% Methanolic Extract of Sonchus oleraceus L.

  • Yin, Jie;Heo, Seong-Il;Jung, Mee-Jung;Wang, Myeong-Hyeon
    • Food Science and Biotechnology
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    • v.17 no.6
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    • pp.1299-1304
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    • 2008
  • The potential antioxidant activities of different fractions from a 70% methanolic (MeOH) extract of Sonchus oleraceus were assayed in vitro. All of the fractions exception of n-hexane showed a strong antioxidant activity, especially the ethyl acetate (EtOAc) fraction, which showed the highest 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activity ($IC_{50}=19.25{\mu}g/mL$). The results of hydroxyl radical scavenging activity and a reducing power assay showed concentration dependence, the EtOAc fraction demonstrating a better result than the other fractions at the same concentration in the studies. Additionally, the fractions' total phenolic (TP) contents was measured, phenolic compounds such as tannic acid, p-coumatric acid, quercetin, epicathchin, and kaempferol being detected by high performance liquid chromatography (HPLC). Meanwhile, a regression analysis revealed a moderate-to-high correlation coefficient between the antiradical activity and the TP contents, suggesting that fractions obtained from the 70% MeOH extract of S. oleraceus are of potential use as sources of antioxidant material.

Determination of L-Carnitine in Infant Powdered Milk Samples after Derivatization

  • Park, Jung Min;Koh, Jong Ho;Kim, Jin Man
    • Food Science of Animal Resources
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    • v.41 no.4
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    • pp.731-738
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    • 2021
  • Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.

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

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.2
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    • pp.81-86
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    • 2015
  • A simple analytical method to quantify formaldehyde in water at lower levels (${\mu}g/L$) was developed using a high performance liquid chromatography (HPLC) and acetylacetone as a derivative reagent. Unlike conventional methods, no extraction and/or concentration were required. The derivative reagent was added into samples and reacted for 30 minutes at $80^{\circ}C$ prior to the analysis of formaldehyde using HPLC. The method detection limit and the limit of quantification for this method were 1.6 and $5.0{\mu}g/L$, respectively. This method also achieved high precision (0.6-3.0%) and accuracy (91.6-106.3%). The recovery rates for various environmental samples ranged from 92.0 to 115.2%.

Stimultaneous Determination of Ephedrine Alkaloids in Ephedra sinica and Wolbigachul-tang by High Performance Liquid Chromatography (고성능 액체 크로마토그래피를 이용한 마황 및 월비가출탕 전탕액에서 에페드린류의 동시분석)

  • Song, Miyoung;Kim, Jung-Ok;Leem, HyunHee;Kim, Hojun
    • Journal of Korean Medicine for Obesity Research
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    • v.20 no.2
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    • pp.97-108
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    • 2020
  • Objectives: Ephedra sinica and Wolbigachul-tang which contains Ephedra sinica are used to treat obesity in Korean medicine. The aim of this study was to analyze the quantities of ephedrine alkaloids by high-performance liquid chromatography. Methods: The analysis was performed using a YMC-Triat C18 column with operating at 25℃, and UV detection at 210 nm. The mobile phase used a gradient flow with 0.1% H3PO4 in water and acetonitrile. Specificity, linearity, precision, accuracy, limit of detection, and limit of quantification were measured for validation anaylsis. This method was applied to analyze the quantities of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang. Results: The concentration per Ephedra sinica (gram) of ephedrine and pseudoephedrine in Ephedra sinica decoction are 4.74±0.22 mg and 2.19±0.10 mg, respectively and in Wolbigachul-tang decoction are 6.39±0.34 mg and 2.97±0.21 mg, respectively. The retention time of ephedrine was 23.6 min and that of pseudoephedrine was 25.8 min, and norephedrine and methylephedrine were not detected. Conclusions: In conclusion, analyzed the concentration of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang by the developed validation method.

On-line Trace Enrichment for the Determination of Insulin in Biological Samples Using Reversed-Phase High Performance Liquid Chromatography with Column Switching

  • Lee, Jung-Sook;Lee, Heeyong;Lee, Hye-Suk;Lee, Kang-Choon
    • Archives of Pharmacal Research
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    • v.17 no.5
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    • pp.360-363
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    • 1994
  • Column--swtiching technique with a reversed-phase high performance liquid chromatographic method has been developed for the routine analysis of radioiodinated insulin and its degadation products in biological fluids. The diluted biological samples were loaded onto a precolumn packed with LiChrosorb RP-8 $(25-40{\;}{\mu}m)$ using 0.1% trifuoroacetic acid (TFA) in water as a washing solvent. After valve switching, the concentrated insulins were eluted in the back-flush mode and separated by a W-Porex $C_{18}$ column with a gradient of 0.1% TFA in water and 0.1% TFA in acetonitrile as the mobile phase. The method showed good precision, accuracy and speed with the detection limit of 20 pg/ml. Total analysis time per sample was about 40 min and the coefficients of variation were less than 8, 2%.

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Synthesis, Characterization and Enhanced Selectivity in RP-HPLC of Polar Carbonyl Group Embedded Poly (Vinyl Octadecanoate) Grafted Stationary Phase by Simple Heterogeneous "Graft from" Technique

  • Rana, Ashequl A.;Karim, Mohammad Mainul;Takafuji, Makoto
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.77-82
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    • 2011
  • A new high performance liquid chromatograpgy (HPLC) stationary phase that possesses an internal carbonyl functional group is synthesized by heterogeneous "graft from" method. This new stationary phase, poly (vinyl octadecanoate) grafted silica (Sil-2) is then characterized by different physico-chemical methods such as diffuse reflectance infrared fourier transform, suspension state $^1H$ NMR, solid state $^{13}C$ CP/MAS NMR, $^{29}Si$ CP/MAS NMR, elemental analysis and thermogravimetric analysis. Chromatographic properties of Sil-2 were evaluated under reversed phase condition by separating polycyclic aromatic hydrocarbons (PAHs) and comparing the chromatographic results with those on polymeric as well as monomeric octadecylated silica stationary phases.