• Journal of the Korean Chemical Society
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• v.54 no.5
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• pp.523-532
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• 2010

The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

• Journal of Animal Science and Technology
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• v.65 no.2
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• pp.401-411
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• 2023

Many studies have been conducted to improve technology for semen cryopreservation in pigs. However, computer-assisted analysis of sperm motility and morphology is insufficient to predict the molecular function of frozen-thawed semen. More accurate expression patterns of boar sperm proteins may be derived using the isobaric tags for relative and absolute quantification (iTRAQ) technique. In this study, the iTRAQ-labeling system was coupled with liquid chromatography tandem-mass spectrometry (LC-MS/MS) analysis to identify differentially expressed CM10-fractionated proteins between fresh and frozen-thawed boar semen. A total of 76 protein types were identified to be differentially expressed, among which 9 and 67 proteins showed higher and lower expression in frozen-thawed than in fresh sperm samples, respectively. The classified functions of these proteins included oxidative phosphorylation, mitochondrial inner membrane and matrix, and pyruvate metabolic processes, which are involved in adenosine triphosphate (ATP) synthesis; and sperm flagellum and motile cilium, which are involved in sperm tail structure. These results suggest a possible network of biomarkers associated with survival after the cryopreservation of Duroc boar semen.

• Environmental Engineering Research
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• v.20 no.2
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• pp.127-132
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• 2015

Perfluorooctane sulfonate (PFOS) and Perfluorooctanoic acid (PFOA) are persistent environmental pollutants, extremely stable, and possibly adversely affect human health. They are widely used in many industries and consumer goods, including sunscreen products. These substances are stable chemicals made of long carbon chains, having both lipid- and water-repellent qualities. The research objectives are (1) to find the most effective method for the preparation of semi-liquid samples by comparing solid phase extraction (SPE) and centrifugation after Pressurized liquid extraction (PLE), and (2) to determine the contamination levels of PFOS and PFOA in waterproof sunscreen samples. All sunscreen samples were analyzed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sunscreen samples were purchased from domestic and international brands sold in Thailand. Special chemical properties were considered for the selection of samples, e.g., those found in waterproof, sweat resistant, water resistant, and non-stick products. Considering the factors of physical properties, e.g., operation time, chemical consumption, and recovery percentage for selecting methods to develop, the centrifugation method using 2 mL of extracted sample with the conditions of 12,000 rpm and $5^{\circ}C$ for 1 hour after PLE was chosen. The highest concentrations of PFOS and PFOA were detected at 0.0671 ng/g and 21.0644 ng/g, respectively. Even though present concentrations are found at ng/g levels, the daily use of sunscreen products is normally several grams. Therefore, a risk assessment of PFOS and PFOA contamination in sunscreen products is an important concern, and more attention needs to be paid to the long-term effects on human health.

• Korean Journal of Food Science and Technology
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• v.43 no.6
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• pp.702-710
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• 2011

The occurrence of aflatoxins $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits was investigated. Samples were collected from local markets in Seoul and analyzed by rapid resolution liquid chromatography coupled with tandem mass spectrometry using an immunoaffinity column. The chromatography method was validated for assay of aflatoxins using linearity, accuracy, precision and limit of detection and quantification. The linearity in the concentration ranged from 0.10 to $20{\mu}g/kg$ with $R^2$ > 0.9999. Sample recoveries ranged from 71.1 to 97.2% with relative standard deviations below 4.5% for spiking levels from 1 to $10{\mu}g/kg$. The limits of detection ranged between 0.02 and $0.05{\mu}g/kg$ and the limits of quantification ranged between 0.05 and $0.10{\mu}g/kg$. The levels of aflatoxin $B_1$, $B_2$, $G_1$ and $G_2$ in nuts, their products and dried fruits were $B_1$ 0.10 to $9.94{\mu}g/kg$, $B_2$ 0.08 to $1.54{\mu}g/kg$, $G_1$ 0.04 to $3.21{\mu}g/kg$ and $G_2$ 0.06 to $0.14{\mu}g/kg$.

• Journal of Ginseng Research
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• v.44 no.4
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• pp.552-562
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• 2020

Background: Ginsenosides are the unique and bioactive components in ginseng. Ginsenosides are affected by the growing environment and conditions. In New Zealand (NZ), Panax ginseng Meyer (P. ginseng) is grown as a secondary crop under a pine tree canopy with an open-field forest environment. There is no thorough analysis reported about NZ-grown ginseng. Methods: Ginsenosides from NZ-grown P. ginseng in different parts (main root, fine root, rhizome, stem, and leaf) with different ages (6, 12, 13, and 14 years) were extracted by ultrasonic extraction and characterized by Liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Twenty-one ginsenosides in these samples were accurately quantified and relatively quantified with 13 ginsenoside standards. Results: All compounds were separated in 40 min, and a total of 102 ginsenosides were identified by matching MS spectra data with 23 standard references or published known ginsenosides from P. ginseng. The quantitative results showed that the total content of ginsenosides in various parts of P. ginseng varied, which was not obviously dependent on age. In the underground parts, the 13-year-old ginseng root contained more abundant ginsenosides among tested ginseng samples, whereas in the aboveground parts, the greatest amount of ginsenosides was from the 14-year-old sample. In addition, the amount of ginsenosides is higher in the leaf and fine root and much lower in the stem than in the other parts of P. ginseng. Conclusion: This study provides the first-ever comprehensive report on NZ-grown wild simulated P. ginseng.

• Fisheries and Aquatic Sciences
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• v.23 no.4
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• pp.10.1-10.10
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• 2020

Background: Butaphosphan (BTP) has recently been introduced into the Korean aquaculture sector as a stressattenuating agent. In this study, a sensitive chemical analytical method was established for the detection of BTP in the olive flounder (Paralichthys olivaceus) tissues. Methods: Utilizing a method employing liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS), detection sensitivity, specificity, and precision were satisfactorily established. Temporal changes in the BTP plasma and muscle concentrations were assessed after a single intramuscular injection of BTP (50 and 150 mg/kg) to the olive flounder maintained at 13 ℃ or 22 ℃. Results: High BTP plasma levels were achieved immediately after the injection, and the drug was rapidly eliminated. Additionally, plasma BTP levels were markedly dependent on the elimination rate, which, in turn, seemed dependent on the water temperature, with the drug elimination half-life and mean residence time significantly shorter at 22 ℃ than 13 ℃. Overall, muscle BTP levels were markedly lower than the plasma levels. Notably, muscle levels were not influenced by water temperatures. Muscle BTP concentrations were used to estimate the necessary withdrawal period for drugs used in food fish, with BTP levels maintained far below the possible hazardous limit. Conclusions: In conclusion, the established LC-MS/MS method can be used for BTP residue detection with high sensitivity and reproducibility.

• YAKHAK HOEJI
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• v.57 no.5
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• pp.330-336
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• 2013

"The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

• Journal of Pharmaceutical Investigation
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• v.38 no.1
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• pp.73-78
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• 2008

To evaluate the bioequivalence of two ramipril formulations, a standard 2-way randomized cross-over study was conducted in twenty-six healthy male Korean volunteers. A single oral dose of 10 mg of test formulation $Ramiprin^{(R)}$ (tablet) or reference formulation Tritace $Protect^{(R)}$ (tablet) was administered with one-week washout period. Plasma concentrations of ramipril were assayed over a period of 12 hr with a well validated method using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The values of area under the plasma concentration-time curve, from time zero to last sampling time $(AUC_t)$ and from time zero to time infinity $(AUC_{inf})$ were $77.45{\pm}44.78\;and\;78.96{\pm}45.64$ for test, and $70.30{\pm}42.27\;and\;71.99{\pm}43.55ng\;hr/mL$ for reference formulation, respectively. Similarly, maximum concentration $(C_{max})$ and elimination half-life $(t_{1/2})$ were $65.61{\pm}19.96ng/mL$ and $2.15{\pm}0.75hr$ for test, and $63.63{\pm}25.50ng/mL$ and $2.16{\pm}0.73hr$ for reference formulations, respectively. Time to reach maximum concentration $(T_{max})$ for the test and the reference, were $0.51{\pm}0.22hr\;and\;0.52{\pm}0.18hr$, respectively. The parametric 90% confidence intervals on the mean of the differences between the two formulations (test-reference) of the log-transformed values of $AUC_t\;and\;C_{max}$ were 1.03 to 1.19 and 0.98 to 1.17, respectively. The overall results indicate that the two formulations are bioequivalent and can be prescribed interchangeably.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.201-210
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• 2017

BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

• Korean Journal of Environmental Agriculture
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• v.34 no.2
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• pp.128-133
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• 2015

BACKGROUND: Plant extracts have been used as environment friendly agricultural materials for organic farming in South Korea. However safety evaluation on the plant extracts was not properly tested. The aim of this study was to evaluate safety of the extracts from Melia azedarach, Nerium indicum and Coptis chinensis on cultivating rice. METHODS AND RESULTS: Pant extarcts 300-fold diluted were treated on rice, and residues of M. azedarach, N. indicum and C. chinensis were determined. The analytes from the rice samples were detected by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The method was validated, and good linearities ($r^2=0.995-0.998$), specificity, and recoveries were obtained. Limits of detection were 0.01 mg/kg for all of the target compounds. Recoveries were 79.3-118.3% at 0.1 mg/kg and 75.2-111.5% at 0.5 mg/kg. The residue levels were below 0.030 mg/kg for azadirachtin, 0.320 mg/kg for oleandrin and 1.460 mg/kg for berberine. CONCLUSION(S): The extracts of M. azedarach, N. indicum and C. chinensis contained azadirachtin, oleandrin and berberine as an active ingredient, respectively. The residue of three active ingredients dramatically decreased after treatment in all fruits, stems and roots of rice.