• Analytical Science and Technology
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• v.7 no.1
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• pp.103-114
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• 1994

The elution behaviors of Ni(II), Cu(II), Co(II), and Cr(II) in 1-phenyl-3-methyl-4(2-hydroxy-5-X-phenylazo)-5-pyrazolone, [Pm(2-OH)(5-X)PaPz](X=H, $CH_3$, $NO_2$, Cl) chelates have been studied by reversed phase HPLC. Thirteen metal-[Pm(2-OH)(5-X)PaPz] chelates were prepared and characterized by UV, IR, MS, and ICP spectroscopic methods. These metal-2-hydroxyarylazopyrazolone chelates were successfully separated on Novapak-$C_{18}$ column using methanol/water mixtures as a mobile phases. It was found that the chelates were eluted properly in an acceptable range of the capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the capacity factor(log k') on the volume fraction of water in the binary mobile phase showed a good linearity. Also, there was a good linear dependence of the capacity factor on the liquid-liquid extraction distribution ratio($D_c$) in methanol-water/n-pentadecane extraction system by the batch method. It suggested that the retention of the chelates in the reverse phase liquid chromatographic system be largely due to the solvophobic effect.

• Journal of Food Hygiene and Safety
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• v.21 no.3
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• pp.153-158
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• 2006

The contamination levels of 3-MCPD(3-Monochloropropane-1,2-diol) and 1,3-DCP(1,3-Dichloro-2-Propanol) in soy sauce, sauces was monitored. 105 samples were collected from June 2005 to August 2005 in Gyeonggi-do. 3-MCPD and 1,3-DCP were analyzed by GCMSD. As results, the detection range of 3-MCPD concentration was between 0.02 mg/kg and 0.27 mg/kg in soy sauce. However any samples were not detected with 1,3-DCP. The contaminated rates of 3-MCPD in soy sauce was 17.1%. Soy sauce is the representative vegetable protein hydrolyzed food. The reliable analytical method f3r the toxic 3-MCPD and 1,3-DCP in Soy sauce has been studied. The derivatization studies of 3-MCPD and 1,3-DCP were performed mainly as Silylation with BSA(N,O-Bis(trimethylsilyl)-acetamide). The retention times of derivative, BSA-MCPD, BSA-DCP were 11.30 and 10.12 minutes.

• Journal of Applied Biological Chemistry
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• v.56 no.3
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• pp.131-135
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• 2013

Jaeumganghwa-tang (JGT) is a traditional herbal medicine used for chronic bronchitis and inflammatory diseases. The variation in the amount of bioactive components of JGT and its fermentation JGT with ten species of microorganism was investigated via high performance liquid chromatography coupled with diode array detection (HPLC-DAD). Simultaneous qualitative and quantitative analysis of eight bioactive compounds; 5- hydroxymethylfurfural (5-HMF), paeoniflorin, nodakenin, hesperidin, nodakenetin, palmatine, berberine and glycyrrhizin were achieved by comparing their retention times ($t_R$) and UV spectra with those of the standard compounds. In the result, the paeoniflorin amount was 6.95 mg/g that as a main compound in JGT. The amount of nodakenetin was the highest in the fermented-JGT with Lactobacillus fermentum KFRI 145 ($0.47{\pm}0.01mg/g$), which was increased by 2,250% compared to that in non-fermented JGT ($0.02{\pm}0.00mg/g$). In the fermented JGT using Lactobacillus acidophilus KFRI 162, most components were increased than non-fermented JGT, except paeoniflorin and hesperidin.

• Analytical Science and Technology
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• v.10 no.5
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• pp.315-324
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• 1997

The retention behaviors of 16 PAHs and 4 nitro-PAHs were studied with several parameters involved numbers of carbon atoms, F factor, aqueous solubility, L/B ratio, and numbers of interfering hydrogen atom pairs on the chemical structures of PAHs by using reversed-phase liquid chromatography/diode array detection method (RPLC/DAD) and gradient elution method. It was obtain that the log k' for most of PAHs with increasing the number of carbon and the F factor in their molecules. Chromatographic retention of PAH isomers and nitro-PAHs were examined with aqueous solubility, L/B ratio and number of interfering hydrogen atom pairs. As a result of comparison with these factors and retention times, it was found that those solutes having larger aqueous solubilities and greater L/B ratios were retained longer on stationary phase. This tendency was also occured in the molecules having the more number of interfering hydrogen atom pairs. Detection limits of PAHs which were obtained with three times measurements by RPLC/DAD were in the range of 100~500ng/mL and method detection limit(MDL) for water sample were in the range of 0.1~0.5ng/mL.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.553-557
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• 2011

Garlic specific organic compounds were separated and purified using a recycling preparative high-performance liquid chromatography (HPLC) from blanched garlic cloves. Identification of the compounds involved comparing the previously reported HPLC retention times as well as other identification methods including $^1H$- and $^{13}C$-nuclear magnetic resonance and liquid chromatography-mass spectrometry. The yields of garlic specific organic compounds were 12.2, 42.5, 1.6, 1.2, and 4.8% on wet weight basis of garlic for alliin(S-allyl-L-cysteine sulfoxide), isoalliin(S-1-propenyl-L-cysteine sulfoxide), ${\gamma}$-glutamyl-S-allylcysteine, ${\gamma}$-glutamyl-S-1-propenylcysteine and ${\gamma}$-glutamyl-phenylalanine, respectively. All the compounds, except for ${\gamma}$-glutamylphenylalanine, contained sulfur.

• Analytical Science and Technology
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• v.7 no.3
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• pp.379-386
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• 1994

The elution behaviors in reversed-phase liquid chromatography were investigated thermodynamically for 2-hydroxy-arylazopyrazolone chelates with Ni(II), Cu(II), Co(III), Cr(III) on Novapak $C_{18}$ column. There was a good linear dependence of the capacity factor(k') on the variations of column temperature in van't Hoff plot. From this result, it was confirmed that the retention mechanism of these chelates in the reversed phase liquid chromatography system was invariant under the condition of various temperatures. For the most cases of the chelates studied, the dependence of capacity factor(1n k') on enthalpy$(-{\Delta}H)^{\circ}$, calculated by van't Hoff plot showed a good linearity(r=0.980~0.999) except [Pm(2-OH_(5-Cl)PaPz](r=0.787) and also the compensation temperatures(${\beta}$) showed constant values. The range of compensation temperature values calculated from the slope of $-{\Delta}H^{\circ}$ vs 1n k' plots was 374.3~806.9K. It was suggested that the retention of metal-2-hydroxy-arylazopyrazolone chelates in the reversed phase liquid chromatography system was largely affected by the hydrophobic effect.

• Analytical Science and Technology
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• v.7 no.3
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• pp.339-347
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• 1994

A multicolumn system consisted of two valve(10-port and 6-port valve)-three column (28% DC 200, SP 1700 and Chromosorb 102 column) was developed. Nine natural gas components composed of $N_2$, $CH_4$, $CO_2$, $C_2H_6$, $C_3H_8$, $i-C_4H_{10}$, $n-C_4H_{10}$, $i-C_5H_{12}$ 및 $n-C_5H_{12}$ completed all the baseline separation within 18 minutes. The accuracy and the precision of this system was tested. The retention times and the peak areas were determined with a repeatability between 0.02 and 0.16%, and less than 1%, respectively. Calibration curves for natural-gas components were plotted by the partial pressure injection method of pure gases, and good linear relationships for each component were presented. By using these calibration curves the accuracy of the multicolumn system compaired with that of the single column system for a certified standard gas of natural gas. As a result, relative error in the single and the multicolumn system was less than 0.5% and 0.04%, respectively. The result of application of this system in the analysis of importing LNG composition showed that the heating values calculated by the multicolum system were estimated lower compared with those calculated by the single column system and consequently, the importing price of LNG was able to be cut down.

• Analytical Science and Technology
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• v.27 no.4
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• pp.201-212
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• 2014

Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted in consumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extraction and quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumer products as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of a bag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of the standard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standard curves for all 18 PAHs were obtained with $R^2$ above 0.999. Precisions of the retention times and the peak areas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. The recoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solvents such as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymer samples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and 1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three samples while 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations of maximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are needed to decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstrate cases that the clean up is required.

• Journal of Ginseng Research
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• v.33 no.1
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• pp.8-12
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• 2009

A simple gradient HPLC method for rapid determination of major ginsenosides ($Rg_1$ and $Rb_1$) and unique ginsenoside (Rf) of Korean ginseng (Panax ginseng C.A. Meyer) was developed. Within 50min, three ginsenosides have been separated and identified on $\mu$-Bondapak $C_{18}$ column ($3.9{\times}300\;mm$, $10{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. The method was validated in terms of linearity, accuracy, and precision. The correlation coefficients ($r^2$) for calibration curves of ginsenosides were over 0.9997. The developed HPLC method was successfully applied to the analysis of ginseng samples and the recoveries of ginsenosides were in the range of $101.1{\sim}115%$ with RSD<3.2%. The developed method could be used for rapid evaluation of the ginsenosides $Rg_1$, $Rb_1$, and Rf.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.50 no.spc1
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• pp.181-186
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• 2005

This experiment was conducted to know the appropriate methods for extraction and determination of rutin contained buckwheat plants. The efficient HPLC analytical condition of rutin contained buckwheat plants was developed. The gradient elution employed a $250mm\times4.6mm$ i.d. Tosoh ODS 120T column. The gradient system was used two mobile phases. A gradient elution was performed with mobile phase A, consisting of $2\%$ Acetic $acid-45\%$ Acetonitrile, and mobile phase B, comprising $2\%$ aqueous acetic acid, and delivered at a flow rate of 1mL/min as follows: 0-18 min, $50-100\%$ A; 18-20 min, $100-50\%$ A; 20-22 min, $50\%$ A. The UV detection wavelength was set at 355 nm. The limit of detection (LOD) for rutin standard compound was 20 ng/mL. And, the higher content of rutin in the extracts was obtained by $80^{\circ}C$ reflex extraction for 120 min. from plants of buckwheat using ethanol.