• Analytical Science and Technology
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• v.27 no.2
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• pp.92-99
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• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

• Korean Journal of Food Science and Technology
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• v.38 no.2
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• pp.309-312
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• 2006

Aflatoxin $B_1$ in 70 retail samples, including 40 food-grade peanut (28 domestic, 12 imported) and 30 peanut butter (12 domestic, 18 imported) samples, was analyzed by high-performance liquid chromatography (HPLC) with fluorescence detection (FD), and positive samples were confirmed using HPLC with mass spectrometry (MS). Recoveries of aflatoxin $B_1$ spiked at 2 ppb exceeded 80% in both commodities. Detection limits for aflatoxin $B_1$ by HPLC-FD and MS analysis were 0.8 and 0.1 ppb, respectively. Four domestic and six imported peanut samples contained detectable levels of aflatoxin $B_1$ with means of 19 and 32 ppb, respectively. Aflatoxin $B_1$ was found in two domestic and three imported peanut butter samples with mean aflatoxin $B_1$ of 10 and 12 ppb, respectively. Peanut commodity showed more frequent aflatoxin $B_1$ contamination compared to its processed peanut butter product, and levels of aflatoxin $B_1$, especially in imported peanuts, were significantly (p<0.05) higher than those of other commodities. These results suggest peanut and peanut butter are not major contributors to dietary intake of aflatoxin $B_1$ in South Korea.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.75-83
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• 2017

The single residue analytical method was developed for determining fungicide pencycuron residues in various agricultural commodities with high-performance liquid chromatography (HPLC). Pencycuron residue was extracted with acetone from representative crops such as Korean cabbage, apple, brown rice and green pepper. After ethyl acetate/n-hexane partition and subsequent clean-up with silica gel chromatography, pencycuron residue was quantified by reversed phase HPLC with UV detection at 240 nm. The suspected residue of pencycuron was confirmed using selected-ion monitoring (SIM) LC/mass spectrometry (MS). Instrumental limit of quantitation (ILOQ) and method LOQ (MLOQ) were set at 2 ng and 0.02 mg/kg, respectively. Overall recoveries of pencycuron from different crop samples fortified at three levels (MLOQ, 10MLOQ, 100MLOQ) were 72~108%. This proposed method could be useful as official analytical method for quantification of pencycuron residues in agricultural commodities.

• Proceedings of the Plant Resources Society of Korea Conference
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• 2010.10a
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• pp.20-20
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• 2010

Panax ginseng C.A Meyer is frequently taken orally as a traditional herbal medicine in Asian countries. The major components of ginseng are ginsenoside, which are pharmaceutical activity. The six major ginsenosides, including Rb1, Rb2, Rc, Rd, Re and Rg1 account for 90% of total ginsenosides. Even though the minor ginsenosides, including Rg3, Rh2 and compound K has high pharmacetical activities, the price of minor ginsenosides is too high. Therefore we isolated the gypenoside V and made it converted to minor ginsenosides. In the plant Gynostemma pentaphyllum Makino, gypenosdie V was presented as dominant saponin (content about 2.4%), and was similar to protopanaxadol type ginsenosides such as ginsenoside Rb1. In this study, we confirmed that the coversion of gypenoside V to minor ginsenosides after using the various treatment such as heating, acid treatment, commercial edible enzyme, and lactobacillus. Consequently, we optimizied the transformation of gypenoside V to minor ginsenoside using Thin Layer Chromatography (TLC), High Performance Liquid Chromatography (HPLC), Time-of-flight Mass Spectrometry (LC/TOF/MS).

• Korean Journal of Medicinal Crop Science
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• v.27 no.3
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• pp.208-217
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• 2019

Background: In the present study, we identified two cytotoxic compounds from the root of Rumex crispus L. using a bioassay-based method. Methods and Results: Compared with the other fractions, the diethyl ether ($Et_2O$) fraction of R. crispus root extract exhibited the strongest of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging effect [scavenging concentration 50% $(SC_{50})=63.8{\pm}1.47{\mu}g/m{\ell}$], nitric oxide (NO) production inhibitory effect on the mouse macrophage cell line RAW264.7 [inhibitory concentration 50% $(IC_{50})=60.9{\pm}7.52{\mu}g/m{\ell}$] and cytotoxicity effect on the human hepatoma cell line, HepG2 [lethal concentration 50% $(LC_{50})=115.4{\pm}1.86{\mu}g/m{\ell}$]. According to the bioassay-based method, two cytotoxic compounds were purified from the $Et_2O$ fraction by using column chromatography and preparative high performance liquid chromatography (prep-HPLC). These two compounds were identified as parietin and chrysophanol by using nuclear magnetic resonance (NMR) and liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS). In addition, both parietin and chrysophanol exhibited a cytotoxicity effect on HepG2 cells, their $LC_{50}$ values were $169.1{\pm}17.67{\mu}M$ and $111.5{\pm}6.62{\mu}M$, respectively. Conclusions: Parietin and chrysophanol isolated from the $Et_2O$ fraction of the R. crispus root extract showed cytotoxicity in HepG2 cell.

• Analytical Science and Technology
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• v.29 no.5
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• pp.234-241
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• 2016

The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R²>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.

• Food Science of Animal Resources
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• v.39 no.6
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• pp.966-979
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• 2019

Muscle-based by-products are often undervalued although commonly reported having a high amount of natural bioactive peptides. In this study, elastin was isolated from the protein of broiler hen skin while its hydrolysate was prepared using Elastase. Assessment of antioxidative properties of elastin-based hydrolysate (EBH) was based on three different assays; 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH) radical, 2,2'-azinobis (3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical and metal chelating ability. The EBH was purified further using ultrafiltration, gel filtration and Reverse- Phase High-Performance Liquid Chromatography (RP-HPLC). The IC₅₀ of ABTS radical activities for EBH were decreased as EBH further purified using ultrafiltration (EBH III; 0.66 mg/mL)>gel filtration (EB-II; 0.42 mg/mL)>RP-HPLC (EB-II4; 0.12 mg/mL). The sequential identification of the peptide was done by matrix-assisted laser desorption/ionization time-of-flight/time-of-flight mass spectrometry (MALDI-TOF/ TOF-MS) of the potent fractions obtained from RP-HPLC (EB-II4). The presence of hydrophobic amino acids (Val and Pro) in the peptide sequences could potentially contribute to the high antioxidant activity of EBH. The sequences GAHTGPRKPFKPR, GMPGFDVR and ADASVLPK were identified as antioxidant peptides. In conclusion, the antioxidative potential from poultry skin specifically from elastin is evident and can be explored to be used in many applications such as health and pharmaceutical purposes.

• Journal of Pharmacopuncture
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• v.15 no.4
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• pp.52-65
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• 2012

Objectives: Toad venom, called Chan-Su, is a traditional Oriental medicine secreted from the auricular and the skin glands of the Bufo bufo gargarizanz Cantor or B. melanosticus Schneider and has been widely used in China, Korea and other parts of Asia for the treatment of pain, heart conditions, and cancer. We examined the concentrations of the main chemical constituents within a commercially available toad venom product and compared the levels for different extraction methods. Methods: Toad venom was extracted using either cold or hot water, ethanol (EtOH), methanol (MeOH), or ethyl acetate (EtOAc), was fractionated using precipitation or reflux, and was then analyzed using thin layer chromatography (TLC), high-performance liquid chromatography (HTLC), and liquid chroma-tography - mass spectrometry (LC-MS). Individual components were identified by comparisons of the retention times, the ultraviolet spectra, and mass spectras and differences in chemical constituents for different solvents and extraction methods are presented. Results: Components with authentic standards, including serotonin and bufodienolides (cinobufagen, bufalin, cinobufalin, and resibufogenin), were detected. The water extract of toad venom contained the greatest amount of serotonin ($75.7{\pm}0.1$ mg/g), but very small amounts of bufodienolides ($3.8{\pm}0.0$ mg/g). In contrast, the use of MeOH or EtOH extraction solutions resulted in 5-26 times higher concentrations of bufodienolides, with only trace amounts of serotonin. The relative and the absolute concentrations of the component also varied based on the extraction method; i.e., EtOH extracts yielded the greatest total amounts of bufodienolides, and EtOAc precipitation had the lowest amounts of bufodienolides. Conclusions: Toad venom consists of serotonin and several bufodienolides, and the choice of solvent to extract chemical the constituents is important as a way to enrich the purported active components for treating different conditions.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.544-552
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• 2011

The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.

• Journal of Environmental Health Sciences
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• v.41 no.5
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.