• Analytical Science and Technology
• /
• v.11 no.3
• /
• pp.213-221
• /
• 1998

The determination of inorganic anions by capillary zone electrophoresis is reported. A ten component synthetic mixture of anions of bromide, chloride, fluoride, nitrite, nitrate, sulfite, sulfate, perchlorate, chlorate and chlorite was separated by the capillary column and detected by indirect UV method. The running buffer contained 5 mM ammonium dichromate, 10 mM ammonium acetate, 20 mM diethylenetriamine, 10% methanol solution at pH 9.3. A potential of 15 kV at the cathode (reversed polarity) was utilized for the separation of inorganic anions. A complete separation of anions was achieved in less then 10 min and the applicabilities of the method for the analysis of real samples was demonstrated. We compare the concentration of anions in toluene inhaled humen's urine and in postmortem bloods obtained by capillary zone electrophoresis and ion chromatograph.

• Korean Journal of Veterinary Service
• /
• v.43 no.4
• /
• pp.261-265
• /
• 2020

Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.4
• /
• pp.601-606
• /
• 2007

The chromatographic behaviors of nucleotides (inosine 5'-monophosphate, uridine 5'-monophosphate, guanosine 5'-monophosphate, and thymine monophosphate disodium salts) on a C18 column were studied with different types of ionic liquids (ILs) as additives for the mobile phase in reversed-phase liquid chromatography (RPLC). Three ILs, 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][BF4]), and 1-ethyl-3-methylimidazolium methylsulfate ([EMIm][MS]), were used. Eluents were composed of water and methanol (90/10%, vol) with the addition of 0.5-13.0 mM of ILs. The effects of the concentration of ILs on retention and separation were investigated and discussed. The results showed that the addition of ILs affects the retention and resolution of the tested compounds. Use of 13.0 mM of [BMIm][BF4] as the eluent modifier resulted in a baseline separation of nucleotides without requiring gradient elution. This study demonstrates that ILs can be potentially applied as a mobile phase modifier in RPLC.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.22 no.6
• /
• pp.815-822
• /
• 1993

This experiment was carried out to determine the separation condition of 1-dimethylaminonaphthalene-5-sulfony(Dansyl) derivatives of amino acids by reverse-phase high performance liquid chromatography with Nova-Pak C18 column. Determined solvent system was solvent A(200mA phosphate buffer pH 6.8 15%, acetonitrile 11%, water 74%) and solvent B(acetonitrile 65%, methanol 28%, water 7%). Linear gradient of solvent B was applied from 12% to 80% for 50min. Complete separation of 20 amino acids including asparagine and glutamine which constitute protein was achieved within 50min. As the detection limit was the range of picomole, the resolution power was excellent. Reproducibility of the retention time was less than mean $\pm$0.05min. According to the above optimum chromatographic conditions, the amino acid composition of some food and human blood was examined. The most affluent amino acid was alanine in human blood, aspartic acid and glutamic acid in soy sauce, alanine and threonine in soy milk and proline in milk and yoghurt.

• Korean Journal of Pharmacognosy
• /
• v.30 no.3
• /
• pp.335-339
• /
• 1999

Separation and quantitative determination of 20-hydroxyecdysone from Achyranthis Radix has been conducted by using HPLC method. 20-hydroxyecdysone in a methanol extract from the raw drug was separated on a reverse phase column using a $CH_3CN-H_2O\;(18:82)$ solvent system and the average content is $0.0931{\pm}0.0048%$. For the preparation of authentic standard, we isolated 20-hydroxyecdysone from the roots of Achyranthes fauriei by $SiO_2$ and RP-18 column chromatography.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.46 no.4
• /
• pp.309-316
• /
• 2001

Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

• Archives of Pharmacal Research
• /
• v.26 no.9
• /
• pp.763-767
• /
• 2003

The differences in pharmacokinetic behavior and tissue distribution of verapamil and its enantiomers were investigated in rats. In high-performance liquid chromatographic method, an achiral ODS column (150 mm $\times$ 4.6 mm i.d.) with the mobile phase consisting of methanol-water (73:30, v/v) was used for the determination of the concentration for racemic verapamil, and a Chiralcel OJ column (250 mm$\times$4.6 mm i.d.) with the mixture of n-haxane-ethanol-triethylamine (85:15:0.2, v/v/v) as mobile phase was used to determine the concentrations of verapamil enantiomers. A fluorescence detector in the analytical system was set at excitation and emission wavelengths of 275 nm and 315 nm. The differences between enantiomers were apparent in the pharmacokinetics in rats. The area under the concentration-time curve (AUC) of S-(-) verapamil was higher than that of R-(+) verapamil. The half-distribution time ($T_{1/2(\alpha)}$) of S-(-) verapamil which distributing to tissue from blood was shorter than that of R-(+) verapamil, but the elimination half-time ($T_{1/2(\beta)}$) was longer in rat following oral administration of racemic verapamil. At 1.3 h after oral administration of racemic verapamil, however, there were no significant differences between enantiomers for the distributions in major tissues such as heart, cerebrum, cerebellum, liver, spleen and kidney.

• Journal of the Korean Chemical Society
• /
• v.36 no.5
• /
• pp.697-708
• /
• 1992

Liquid Chromatographic behavior of Ni(II) in Isonitrosoethylacetoacetate Imine(IEAA-NR), Ni(IEAA-NH)(IEAA-NR)(R = H, CH_3, C-2H_5, n-C_4H_9, C_6H_5-CH_2) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of Ni(IEAA-NH)(IEAA-NR) chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It was fo$und that metal chelates were properly eluted in an acceptable range of capacity factor value(0{\le}logk'{\le}1). The dependence of the logarithm of capacity factor (k') on the volume fraction of water in the binary mobile phase as well as on the liquid-liquid extraction distribution ratio (Dc) in methanol-water/n-alkane extraction system showed the good linearties, and the dependence of the logarithm of capacity factor (k') on the column temperature and on the enthalpy exhibited the good linearties, and the compensation temperature ({\beta}) from the slope was 773.47{\circ}K. It was suggested that the retention of metal chelates was largely affected by the hydrophobic effect.

• Archives of Pharmacal Research
• /
• v.20 no.5
• /
• pp.486-490
• /
• 1997

A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with (S)-(-)-${\alpha}$-methyl-benzyl isocyanate, the diastereomeric derivatives were resolved $(R_s=1.59)$ on $5{\mu}M$ octadecylsilan column using 47% methanol as a mobile phase with fluorescence detection. The detection limit of each enantiomer was 10 ng/ml (S/N=3).

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.43 no.4
• /
• pp.209-213
• /
• 1998

The sesaminol glucosides in 80% EtOH extract from sesame seeds were separated by high performance liquid chromatography (HPLC). A HPLC system using a Develosil ODS-5 column and gradient elution system from 30% to 80% methanol was selected for separation and quantitative determination of sesaminol triglucoside, sesaminol diglucoside, and sesaminol monoglucoside. Quantitative analyses for these sesaminol glucosides, sesaminol triglucoside, sesaminol diglucoside, and sesaminol monoglucoside were determined on the basis of standard curve of sesaminol glucosides. Sesaminol triglucoside, sesaminol diglucoside and sesaminol monoglucoside contents of the seed of one Korean sesame cultivar, Danbaekggae, were 56.4 mg/100g, 9.6 mg/100g, and 7.5 mg/100g, respectively. The most abundant aglycon of lignan glucosides in sesame seed was sesaminol triglucoside