• The Korean Journal of Pesticide Science
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• v.9 no.4
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• pp.303-310
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• 2005

This study was performed to examine analytical method of a quinolone compound, oxolinic acid in paddy soil by HPLC coupled with UV detector. Two types of soil texture in different regions were used for this experiment. Oxolinic acid was extracted by a 4 M-KOH : MeOH(1 : 3, v/v) mixtures and acidified followed by liquid-liquid partitioning in dichloromethane. Dichlormethane layer was dehydrated, evaporated and analyzed by HPLC (262 nm). Retention time was 10.2 min. The standard calibration curve of oxolinic acid showed linearity ($r^2>0.999^{**}$, y=378.99x+135.08) in the range of $1{\sim}40$ ng. The mean recoveries, evaluated from fortified soil samples at two concentration levels of 0.2 mg/kg and 1.0 mg/kg, were $90.9{\pm}4.52%$(C.V. 4.97%) and $95.0{\pm}0.23%$(C.V. 0.24%) for soil 1 and $92.2{\pm}1.15%$(C.V. 1.25%) and $93.1{\pm}0.31%$ (C.V. 0.33%) for soil 2, respectively The detection limits of two types of soils were same as 0.05 ppm. Overall, the present analytical method of oxolinic acid by HPLC coupled with UV detector seems to be used reasonably.

• Food Science and Preservation
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• v.22 no.4
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• pp.553-558
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• 2015

The aims of this study was to optimize the extraction conditions of sinigrin from Dolsan leaf mustard. Dolsan leaf mustard (Dolsan-eup, Yeosu-si) harvested during at May 2014 was used for sinigrin extraction. After the extraction of sinigrin using 50% $CH_3CN$, 10% $NH_4Cl$, 60% $CH_2OH$, and 70% $CH_3OH$, the sinigrin content was measured by HPLC analysis. The results showed that sinigrin content was highest with 50% $CH_3CN$ solvent extraction and UV detector sensitivity was greater at 228 nm rather than at 242 nm. The sinigrin concentrations of leaf, stem and root with 50% $CH_3CN$ extraction were 345 ppm, 728 ppm, and 539 ppm, respectively. After extraction of the different parts of Dolsan leaf mustard, The standard retention time by HPLC analysis of sinigrin content was 2.054, 2.032, 2.059, and 2.035 min from the root, stalk, and leaf, respectively. On the other hand, HPLC analysis showed that the leaf extracts contained glucoraphanin, one of glucosinolates. The optimum time and extraction solvent for the sinigrin extraction from Dolsan leaf mustard was found to be 24 hr with 50% $CH_3CN$ solvent. In addition, opotimum UV detector k at 228 nm. These results showed that the optimum extraction conditions for Dolsan leaf mustard were 24 hr extraction with 50% $CH_3CN$ solvent. In addition, the optimum wavelength of UV detector was determined to be 228 nm for sinigrin analysis. Therefore, this study could provide a useful information for sinigrin extraction and its systematic analysis during the storage.

• Korean Journal of Veterinary Service
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• v.29 no.3
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• pp.317-330
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• 2006

This study was conducted to develop the analytical method about simultaneous determination for synthetic antimicrobials in muscle by high performance liquid chromatography - mass selective detector (HPLC- MSD). Solid phase extraction (SPE), matrix solid phase dispersion (MSPD) and liquid-liquid extraction (LLE) have been adapted as pretreatment procedures for HPLC- MSD. Among various solvent tested, methanol was chosen for extraction of synthetic antimicrobials in muscles. For the optimized response, the values of various MS parameters including fragment voltage, drying gas flow, nebulizer pressure, drying gas temperature were verified. The average recovery rates using MSPD and SPE for muscles of bovine and pork were 78.9-127.1% and 78.3-121.7%, respectively. This method was verified the satisfactory performance for fourteen synthetic antimicrobials excepting carbadox in muscle of pork as detection limit of $0.05{\mu}g/g$ on API/ES SIM mode.

• Applied Biological Chemistry
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• v.39 no.1
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• pp.84-88
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• 1996

To determine brassinolide in rice(Oriza sativa L.) using HPLC equipped with fluoresence detector, a highly sensitive fluorescence reagent. 1-cyanoisoindole-2-m-phenylboronic acid, was synthesized from the reaction of o-phthaldehyde, m-phenylboronic acid and KCN, then was reacted with brassinolide. The formation ratio of brassinolide boronate exhibited 90% up at the ratio of $20\;:\;1({\mu}g/{\mu}g)$ of 1-cyanoisoindole-2-m-phenylboronic acid and brassinolide respectively. The detection limit of brassinolide boronate with fluoresence detector was 0.16 ng. Brassinolide was detected in heading stage(biomass : 10 g) and panicle formation stage(biomass : 100 g) of the rice(Oryza sativa L.) with quantity of $0.8\;{\mu}g\;and\;0.2\;{\mu}g$respectively. However, brassinolide was not detected in blooming and elongation stage.

• Analytical Science and Technology
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• v.19 no.6
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• pp.519-528
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• 2006

An analytical method for the determination of thyroid hormones in urine samples has been studied by using solid-phase extraction and high-performance liquid chromatography/diode array detector/electro-spray mass spectrometry. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 100 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile, and UV spectra and mass fragment could be confirmed. The extraction recoveries of thyroid hormones in the urine samples (pH 3) were in the range of 89.0-113.1% with solid-phase extraction by C18, followed by elution with 4 ml of methanol/ammonium hydroxide (9 : 1). The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.992 to 0.998 and the detection limits of all analytes were obtained in the range of 2-4 ng/ml (3.8-13.0 pmol/ml).

• Toxicological Research
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• v.12 no.2
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• pp.163-169
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• 1996

The focus of this study was to investigate the suitable analytical methods for measurement of sulfamerazine and its metabolite in shrimp hepatopancreas and tail tissue, in addition to the methods for the optimization of solid-phase extraction cartridge conditions and the elucidation of sulfamerazine concentrations in aqueous buffer using HPLC with UV and EC detectors. Compared with UV detector the EC detector appears to be 10 times more sensitive than that of the UV detector. After the shrimp was exposed to 10 ppm sulfamerazine, the accumulation levels of sulfamerazine and its metabolite in tail tissue, which is edible portion, were considerably lower than 0.1 ppm. The data indicate that sulfamerazine continues to be a candidate for use at levels of sulfamerazine concentration used in aquaculture of shrimp.

• Korean Journal of Food Science and Technology
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• v.34 no.6
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• pp.1145-1148
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• 2002

Melatonin, which is a hormone secreted from pineal gland of brain and known to prevent oxidative damages of various tissues, was analyzed in 26 domestic edible plants. For the preparation of melatonin fraction, 50% ethanol extract prepared from lyophilized plant powder was filtered and applied on TLC plate. Melatonin position on TLC developed with acetone was identified by fluorescence light and extracted with methanol. This methanolic fraction was injected into HPLC comprising ODS-A column, fluorescence detector, and mobile phase consisting of a mixture (30 : 70, v/v) of 70% ammonium acetate and methanol at a flow rate of 1.0 mL/min. Melatonin was identified at the retention time of 17 min. Results revealed that celery, leek, broccoli, and cauliflower had higher melatonin contents than others.

• Korean Journal of Food Science and Technology
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• v.32 no.4
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• pp.788-791
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• 2000

The quantitative analysis of chitooligosaccharide was compared to using colorimetry and HPLC method. HPLC method required less than 10mins per sample in analytical time of glucosamine and its the recovery rate was 98.4% (10 mg/ml, w/v). Also there was no the effects of interfering substances(false positive response) by HPLC method. The content of chitooligosaccharide in processed chitooligosaccharide products obtained using HPLC showed lower levels compared to colorimetry. Thus, HPLC method was more sensitive, effective and precise than the colorimetry currently used to determine the glucosamine of chitooligosaccharide.

• YAKHAK HOEJI
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• v.31 no.2
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• pp.112-115
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• 1987

Gypsogenin was derivatized with 2, 4-dinitrophenylhyclrazine prior to analysis with HPLC. Reversed-phase column (Du pont ODS) was used and the mobile phase was acetonitrile and water (60:40). The effluent was detected at 550nm using an U.V. detector and the retention time was approximately 9.2min. The concentration was quantitated by measuring the area and the detection limit was 0.2$\mu\textrm{g}$.

• Korean Journal of Food Science and Technology
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• v.31 no.1
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• pp.30-35
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• 1999

A simple, rapid, efficient method is for extraction of 13 synthetic water-soluble food colours (Tartrazine, Amarnth, Indigo carmine, New coccine, Sunset yellow FCF, Allura red AC, Eosine, Fast Green FCF, Brilliant Blue FCF, Erythrosine, Acid red, phloxine, Rose Bengal) by polyamide resin and for their quantitative by high performance liquid chromatography (HPLC). Colours (coal-tar dyes) were extracted with polyamide resin and then determinated by HPLC. The HPLC conditions using a reverse phase partition type column $(Nova-pak\;C_{18})$, photodiode array (PDA) detector and 1% Ammonium acetate / 60% acetonitrile in water as eluent, were acceptable for various kinds of colorants. By the use of the proposed method, a survey of coal-tar dyes was carried out on 20 samples and that were detected $4.76{\sim}133.47\;ppm$.