• Journal of the Korean Magnetic Resonance Society
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• v.22 no.2
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• pp.26-33
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• 2018

Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.

• Journal of the Korean Society of Clothing and Textiles
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• v.37 no.6
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• pp.827-836
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• 2013

Indigotin, indirubin, berberine, palmatine, alizarin, and purpurin are major pigments of indigo plant, Phellodendron bark, and madder. The six pigments were examined using the HPLC-DAD-MS instrument for the purpose of the simultaneous detection of the pigments in a single sample run. The HPLC-DAD-MS method examined the individual pigment solutions in DMSO, a solution containing 6 pigments, and the DMSO extract of the silk dyed with a dye solution of 5 pigments excluding indirubin. The retention times of the HPLC chromatograms, ${\lambda}_{max}$ of the uv-vis absorption bands in the DAD analyses, and the molecular ions detected for the compound peaks in the MSD analyses were consistent throughout the analyses of individual pigment solutions, mixed pigment solutions, and dye extracted from silk dyeing. The developed instrumental method of the simultaneous detection of six pigments can identify dye in an exhumed textile if the textile is dyed using any one (or multiple) pigments of indigo, Phellodendron bark, or madder plant.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.149-159
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• 2011

Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 ($4.6{\times}250$ mm) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 mg/kg in apple to 97.9% for a 0.02 mg/kg in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 mg/kg in soybean to 9.7% for a 0.02 mg/kg in Chinese cabbage. Quantitative limit of bentazone was 0.02 mg/kg in representative five crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of bentazone in agricultural commodities.

• Proceedings of the KSEEG Conference
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• 2007.04a
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• pp.364-366
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• 2007

• Journal of the Korean Society of Food Science and Nutrition
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• v.29 no.5
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• pp.747-751
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• 2000

This study was carried out to improve the analysis method of gingerol compounds from ginger (Zingiber officinale Roscoe). Pungent components of ginger were extracted by acetone and lisolated by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) with LiChrosorb RP-18 column. Three homologues of gingerols were identified by HPLC-mass spectrometry (LC/MS) and nuclear magnetic resonance (NMR). The contents of [6]-, [8]- and [10]-gingerols in three homologues identified were 635.3 mg%, 206.6 mg% and 145.7 mg% in raw ginger, and were 418.2 mg%, 142.6 mg% and 103.3 mg% in ginger paste, respectively.

• 대한임상약리학회:학술대회논문집
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• 2006.11a
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• pp.83-83
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• 2006

• Journal of Food Hygiene and Safety
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• v.25 no.1
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• pp.30-35
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• 2010

It has been elucidated desmethylsibutramine in food, that is an analogue of sibutramine used for anti-obesity drug. After separating and purifying in food samples, it was analyzed and identified by the instrument such as HPLC/PDA, HPLC/MS, HPLC/MS/MS and NMR. To analyze sibutamine and desmathylsibutramine in foods, they were analyzed and identified by HPLC/PDA after extracting in dichloromethane, filtering, concentration and diluting in methanol. The overall recoveries were ranged from 87% to 91% and the limit of quantitation was $2.5\;{\mu}g/kg$. As results, sibutramine and desmethylsibutramine was not detected in all the selected 54 food samples.

• Natural Product Sciences
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• v.19 no.1
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• pp.20-27
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• 2013

A simple high performance liquid chromatography - diode array detector (HPLC-DAD) method has been developed and validated for simultaneous determination of the six components (cinnamic acid, cinnamaldehyde, eugenol, atractylenolide I, atractylenolide III, and ergosterol) in Oryeongsan. In addition, identification of six marker compounds was conducted by a LC-MS/MS analysis. The six compounds in Oryeongsan were separated on Shishedo $C_{18}$ column (5 ${\mu}m$, $4.6{\times}250$ mm) at a column temperature of $30^{\circ}C$. The mobile phase was a mixture of 0.1% trifluoroacetic acid (TFA) water and acetonitrile employing gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205, 250, 280, and 330 nm. The developed method had good linearity ($R^2$ > 0.9997) and the limit of detection (LOD) and limit of quantification (LOQ) were observed within the ranges 0.01~0.15 and 0.05~0.45 ${\mu}g/mL$, respectively. The relative standard deviation (RSD) values of intra- and inter-day testing were indicated that less than 3% and 90.31~103.31% of accuracy. The results of recovery test were 90.56~106.72% and RSD range was measured from 0.84 to 2.95%. In conclusion, this HPLC-DAD method has been successfully applied to the simultaneous determination of six compounds in Oryeongsan samples.

• The Korean Journal of Pesticide Science
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• v.15 no.2
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• pp.125-133
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• 2011

Ametryn is used in USA, China, and Japan, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of ametryn were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for ametryn residue in crops using HPLC-UVD/MS. Ametryn residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover ametryn from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The ametryn was quantitated by HPLC with UVD, using a Tosoh ODS 120T ($4.6{\times}250$ mm) column. The crops were fortified with ametryn at 2 levels per crop. Mean recovery ratio were ranged from 83.7% for a 0.2 mg/kg in soybean to 91.1% for a 1.0 mg/kg in hulled rice. The coefficients of variation were ranged from 1.2% for a 1.0 mg/kg in hulled rice to 3.6% for a 1.0 mg/kg in soybean. Quantitative limit of amatryn was 0.02 mg/kg in representative 5 crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of ametryne in agricultural commodities.

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.