• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.236-246
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• 2016

The aim of this study was to develop an analytical method for the determination of pyribencarb and its metabolite KIE-9749 in agricultural commodities. The experiment was performed with a range of concentrations $0.05{\sim}2.5{\mu}g/g$ in apple, green pepper, potato, hulled rice, soybean, pear, peach, grape and cucumber. Each samples were extracted with acetone and cleaned by dichloromethane/saline water partition and purified with Florisil solid phase extraction (SPE) cartridge and aminopropyl SPE cartridge. Pyribencarb and KIE-9749 were separated and quantified by HPLC/UVD at 265nm using acetonitrile and water as mobile phase. The recoveries of pyribencarb and KIE-9749 were within 78.3~108.4% and 73.9~113.7% with RSD below 12.2% and 15.0%, respectively. The limits of quantification (LOQ) were both $0.05{\mu}g/g$. LC/ESI-MS/MS was optimized for confirmation of residue identity.

• 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.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.6
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• pp.958-964
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• 2002

To select the irradiation-induced marker components from volatile flavor compounds in irradiated chicken, and complement the extraction problems of liquid continuous extraction (LLCE) method, the volatile compounds of irradiated (0,1,3,5 and 10 kGy) chicken were analyzed by Purge and Trap (P&T) and gas chromatography/mass spectrometry (GC/MS) methods. A total of 119 compounds were detected in irradiated chicken, and these compounds were composed mainly of 7 aldehydes,22 ketones,8 alcohols,30 esters,36 hydrocarbons,8 aromatic compounds and 8 miscellaneous compounds. Among these, only 21 compounds were detected in both LLCE and P&T methods, and the 98 other were detected in omly P&T method. Among volatile compounds detected in irradiated chicken, only 3 compounds such as hexene (r=0.96, p<0.01), propanol (r=0.93, p<0.05) and 1,3-bis(1,1-dimethylethyl) benzene (r=0.96, p<0.05) were newly selected as marker compounds in irradiated chicken by P&T method, which showed significant and high positive correlation coefficient in the change of relative concentration according to the increment of irradiation dosage.

• Korean Journal of Food Science and Technology
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• v.13 no.1
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• pp.57-66
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• 1981

An effective method for isolation of the major components of ginseng saponin such as $ginsenoside-Rb_{1},\;-Rb_2,$ -Rc, -Rd, -Re and $-Rg_1$, and the minor components such as ginsenoside-Rf, $-Rg_2,\;and-Rh_1$, was developed and reported in previous papers (J. Korean Agr. Chem. Soc., 23(4), 199 and 206(1980) The conditions and procedures used for isolation and identification for ginsenosides described in the previous papers were not sufficient enough for clean separation of minor components, $ginsenoside-Rh_1,\;and-Rh_2$. In this work, modifications in extraction method and in mobile phase for HPLC were attempted. It was found that application of ethyl acetate extraction at $60^{\circ}C$ for 3 hr on crude saponin resulted in a removal of diol group saponin from crude saponin which made it possible for using higher portion of acetonitrile in mobile phase. The mixed solvents of acetonitrile : water (92 : 8 and 94 : 6) gave excellent resolution of $ginsenoside-Rh_1\;and\;-Rh_2$.

• Korean Journal of Environmental Agriculture
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• v.36 no.4
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• pp.269-278
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• 2017

BACKGROUND: The objective of this study was to evaluate screening method of residual multi pesticides in dead birds by Orbitrap high resolution mass spectrometry (HRMS) to identify the cause of death for birds. METHODS AND RESULTS: Extraction and clean-up method of residual pesticides in liver of dead birds was used QuEChERS (Quick Easy Cheap Effective Rugged and Safe) and method validations was conducted using liquid chromatography and gas chroamtography with triple-quadrupole mass spectrometer (LC/MS/MS and GC/MS/MS) Also, we were evaluated screening method for the determination of residual pesticides in liver of dead birds by LC and GC Orbitrap Mass Spectrometry. Results of method validations, Correlation coefficients of the matrix matched calibration curves were >0.978, and the method detection limits (MDLs) and limits of quantitation (LOQ) were 2.8~72.1 ng/g (18.4 ng/g on average) and 9.0~230 ng/g (58.5 ng/g on average). The accuracy ranged from 69.1%to 130% (103% on average), and the precision values were less than 14.8%(3.8%on average). The screening of residual pesticides in liver of dead birds by LC and GC Orbitrap HRMS was detected monocrotophos, carbofuran, carbosulfan, deltametrin, benfuracarb, carbofuran, phosphamidon, prochloraz in investigated samples. CONCLUSION: This results showed that accurate mass were extraction of residual pesticides in dead birds by Orbitrap HRMS. It suggested that this screening method is applicable to the residual pesticide analysis for the cause of death as a main tool.

• Journal of Food Hygiene and Safety
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• v.27 no.1
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• pp.37-41
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• 2012

The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

• Journal of Food Hygiene and Safety
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• v.33 no.5
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• pp.354-360
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• 2018

This study presents a method validation for extraction and quantitative analysis of trichothecene mycotoxins in nuts based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach for extraction and enhanced matrix removal (EMR)-lipid-disperive-SPE (d-SPE) cleanup method, with detection and quantification by high-performance liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) in positive- and negative-ion modes. Linearity, precision, and accuracy were validated for LC-MS/MS methods. Results obtained with LC-MS/MS were linear, with correlation coefficient ($R^2$) of 0.998. Limits of detection and quantification for mycotoxins were $0.41-3.57{\mu}g/kg$ and $1.23-10.82{\mu}g/kg$, respectively. Intra- and inter-day precisions (RSD, %) were 0.40-8.44% and 1.93-12.46%, respectively. Results indicated to be rapidly and accurately identifying trichothecene mycotoxins and may be used as a suitable safety management method for nuts and nuts related commodities.

• Food Science and Preservation
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• v.22 no.6
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• pp.859-866
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• 2015

The purpose of this study was to develop a supplemental healthy food that can help prevent high blood pressure-related diseases caused due to the excessive consumption of sodium in salt. This was achieved by using ion-displacement techniques to produce mineral salt with lower sodium content by using fermented brown rice by-products rich in minerals. Mineral salt containing 2019.2 mg/100 g of potassium, 678.5 mg/100 g of magnesium, 48.7 mg/100 g of calcium, and 19.5 mg/100 g of sodium was obtained by fermenting brown rice by-products to create a culture medium for the mineral salt. Mineral salt containing 1769.7 mg/100 g of potassium, 573.6 mg/100 g of magnesium, 35.3 mg/100 g of calcium, and 19.5 mg/100 g of sodium was obtained by filtering and refining the by-product extract of fermented brown rice. The results showed that when the stream velocity of the instrument used for electrolysis was 200 mL/min and the current and the concentration of the reactive liquid in the purified water chamber were higher, the effect of electrolysis was greater. Ion hot water extraction of the fermented brown rice by-products improved by up to 95% and was collected as purified water within 90 min of the reaction time. Chloride ions with pH 7.4 were produced by mixing sodium hydroxide in a purified saline water chamber with electro-analyzed water. The salt produced in this study contained low sodium, 5.7~30%, as compared to 40% sodium content of the normal salt.

• Korean Journal of Medicinal Crop Science
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• v.7 no.1
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• pp.45-50
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• 1999

Timosaponin A III, an active and major compound, was isolated from rhizomes of Anemarrhena asphodeloides. The quantitative analysis of timosaponin AIII was performed by a high performance liquid chromatographic(HPLC) method using ELSD and the useful extraction method for HPLC analysis was examined as well. This HPLC method can be utilized as the standard analytical method for the evaluation of the quality of Anemarrhena rhizoma in the steps of breeding and cultivation. Additionally, the HPLC analysis method can be useful for the evaluation of the quality of Anemarrhena rhizoma sold as a traditional medicine in current markets.

• Applied Biological Chemistry
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• v.40 no.5
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• pp.365-368
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• 1997

This study was carried out to investigate the optimum mashing and maturing conditions for Korean traditional Kanjang(soy sauce) production and to reduce the fermentation period. The effects of maturing time of soy sauce mash, maturing temperature, salt concentration and the ratio of Meju to salt brine on the quality of Kaniang(total nitrogen, pH and color) were examined. Soy sauce pigments and about 90% of N constituents contained in soybean Meju(Koji) in soy sauce mash were degraded and solubilized into liquid portion (soy sauce) of the mash within five days of maturing at $30^{\circ}C$ with the mashing ratio(weight/volume) of 1 : 4 of soybean(as raw soybean) to 20% salt brine. No remarkable effects of soy sauce maturing temperature in the range of $5^{\circ}C{\sim}30^{\circ}$ on the digestion and solubilization of N components and pigment extraction during five days of soy sauce mash maturing were observed. Optimum mashing salt brine concentration for the digestion and solubilization of N components and pigment extraction during soy sauce maturing at $30^{\circ}C$ were observed to be in the range of $15{\sim}20%$. The suitable mashing ratio of Meju to salt brine (wt./vol.) to match N content of the standards of identity of Korean traditional Kanjang(soy sauce) was found to be below 1 : 5.