• Korean Journal of Environmental Agriculture
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• v.42 no.1
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Environmental Agriculture
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• v.42 no.2
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• pp.139-151
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• 2023

Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO₄ (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO₄ and C₁₈ (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R²) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

• Korean Journal of Environmental Agriculture
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• v.41 no.4
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• pp.355-364
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• 2022

BACKGROUND: Pre-harvest interval and decline pattern of thiamethoxam were determined in kiwifruit using liquid chromatography-tandem mass spectrometry (LCMS/MS). The study was carried out to propose import tolerance using OECD maximum residue limit (MRL) calculator for the export promotion of kiwifruit to Taiwan. METHODS AND RESULTS: The thiamethoxam residue in kiwifruit was determined by using the LC-TriQ-MS/MS with the analytical process to set up the import tolerance under greenhouse conditions for Taiwan. Excellent linearity was observed for all of the analytes with a determination coefficient (R²)≥0.99. The limit of quantification was determined to be 0.01 mg/kg for both thiamethoxam and clothianidin in kiwifruit. Linearity was determined from the co-efficient of determinants (R²) obtained from the seven-point calibration curve. The standard calibration curve showed as follows; 1) Site 1 (Gimje): y = 944,406X + 1,583 (R²=0.9995), 2) Site 2 (Goheung): y = 1,356,205X + 934 (R²=0.9983), and 3) Site 3 (Jangheung): y = 1,239,937X - 3,090 (R²=0.9908). The residue of thiamethoxam in the kiwifruit for three decline trials showed the range of 0.35 to 0.56 mg/kg in site 1 (Gimje), 0.24 to 0.55 mg/kg in site 2 (Goheung), and 0.28 to 0.42 mg/kg in site 3 (Jangheung), respectively. However, clothianidin was not detected in all of the treatments. The maximum residual amounts (decline) in the samples, sprayed according to the safe-use standard for thiamethoxam 10% WG in kiwifruit (30 days before harvest, 3 sprays every 7 days) were 0.56 mg/kg in site 1, 0.55 mg/kg in site 2, and 0.42 mg/kg in site 3, respectively. CONCLUSION(S): The import tolerance (IT) of thiamethoxam for kiwifruit may be proposed to be 0.9 mg/kg by using the OECD MRL calculator.

• Analytical Science and Technology
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• v.21 no.1
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• pp.34-40
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• 2008

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitative determination of lercanidipine in human plasma. After addition of internal standard (amlodipine), plasma was precipitated with acetonitrile and the supernatant was evaporated. The residues were dissolved in 50 % acetonitrile and analyzed by LC-MS/MS. Using MS/MS with multiple reaction monitoring(MRM) mode, lercanindipine were selectively detected without severe interference from human plasma. The standard calibration curve for lercanidipine was linear (r = 0.9994) over the concentration range 0.05-20.0 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of lercanidipine was lower than 11.7 % (correlation of variance, CV), and accuracy was between 94.4-114.8 %. This method has been successfully applied to the pharmacokinetic study of lercanidipine in human plasma.

• Analytical Science and Technology
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• v.22 no.1
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• pp.101-108
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• 2009

The bioequivalence of two pioglitazone tablets, Actos$^{(R)}$ tablet (Takeda Chemical Industries, reference drug) and Pioglitazone tablet (Boryung Company, test drug) was evaluated according to the guidelines of Korea Food and Drug Administration. Twenty-eight healthy male Korean volunteers received each medicine (pioglitazone dose of 30 mg) in a $2{\times}2$ crossover study with one week washout interval. After drug administration, blood samples were collected at specific time intervals from 0-36 hours. The plasma concentrations of pioglitazone were determined by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The total chromatographic run time was 5 min and calibration curves were linear over the concentration range of 5-2000 ng/mL for pioglitazone. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. The pharmacokinetic parameters were determined from the plasma concentration-time profiles of both formulations. The primary calculated pharmacokinetic parameters were compared statistically to evaluate bioequivalence between the two preparations. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for Pioglitazone tablet and Actos$^{(R)}$ tablet were log0.9422~log1.1040 and log0.9200~log1.1556, respectively. Based on the statistical considerations, we can conclude that the test drug, Pioglitazone tablet was bioequivalent to the reference drug, Actos$^{(R)}$ tablet.

• Analytical Science and Technology
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• v.21 no.3
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• pp.191-200
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• 2008

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in aquatic environmental samples. Therefore, it required rapidly and certainly analytical method for pharmaceuticals which are existed in environment. In this study, Liquid chromatography/tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) was used to measure the concentrations of 7 pharmaceuticals (quinoxaline-2-carboxylic acid, acetylsalicylic acid, diclofenac-Na, naproxen, ibuprofen, mefenamic acid, talniflumate) from environmental water or aquatic samples simultaneously. Effective sample clean-up by solid-phase extraction (SPE) prior to LC-MS/MS analysis is necessary. For further purification, Mixed Cation eXchange (MCX) and Hydrophilic-Lipophilic Balance (HLB) solid-phase extraction (SPE) cartridges were used to eliminate the remaining interferences. LODs (Limits of Detection) and MDLs (Method Detection Limits) for the spiked sample in fresh water were in the range of 0.05~1.50 pg/mL and 0.17~4.90 pg/mL, respectively. The absolute recovery in the concentration of 1.0 ng/mL were between 81.9 and 116.3%. The acidic pharmaceuticals were detected in concentrations of 0.018~16.925 ng/mL in aquatic environmental samples.

• Analytical Science and Technology
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• v.20 no.4
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• pp.331-338
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• 2007

Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

• Journal of Food Hygiene and Safety
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• v.38 no.6
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• pp.476-482
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• 2023

This study aimed to investigate the acrylamide content in frozen food products after cooking. Twenty samples of bread (Group 1) and 30 samples of processed tuberous and corn vegetable products (Group 2) were selected. Acrylamide levels were quantified using liquid chromatography tandem-mass spectrometry (LC-MS/MS). The frozen food samples were heated using the air fryer cooking method according to the product packaging and were compared to ready-to-eat French fries (Group 3). The results showed that the acrylamide content was the highest in group 3, followed by that in group 2 and group 1. The acrylamide content of all the samples was found to be within the domestic recommended standard of 1 mg/kg. However, when the samples that exceeded EU benchmark level (0.5 mg/kg) were selected and cooked using the deep-fat frying method according to the product packaging, one of them showed the acrylamide content of 1.83 mg/kg, which exceeded the domestic recommended standard. The present study highlights the need for continued evaluation and management to reduce acrylamide contents in frozen foods, as increasing domestic exposure to acrylamide is concerning.

• Journal of Applied Biological Chemistry
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• v.66
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• pp.467-476
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• 2023

Schisandra chinensis (S. chinensis) is a deciduous broad-leaved cave plant belonging to the Schisandraceae family and is widely distributed in East Asia including Korea, Japan, China, and Taiwan. It has been reported that the main components contained in S. chinensis include lignan compounds and triterpenoid compounds. To distinguish the characteristics of S. chinensis by production region of Korea, a discriminant was established by performing metabolite profiling and principal component analysis, a multivariate statistical analysis technique. As a result, 16 types of triterpenoids, 9 types of lignan, and 1 type each of flavonoid, phenylpropanoid, and fatty acid were identified. In addition, through multivariate statistical analysis, it was confirmed that the four groups in Danyang, Moongyeong, Geochang, and Pyeongchang were divided, by applying the s-plot model of orthogonal partial least squares discriminant analysis. Biomarkers were identified: lanostane, cycloartane, schiartane triterpenoid, and dibenzocyclo-octadiene lignan were identified as chemical markers, respectively.

• Molecules and Cells
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• v.46 no.11
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• pp.688-699
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• 2023

We set up this study to understand the underlying mechanisms of reduced ceramides on immune cells in acute rejection (AR). The concentrations of ceramides and sphingomyelins were measured in the sera from hepatic transplant patients, skin graft mice and hepatocyte transplant mice by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Serum concentrations of C24 ceramide, C24:1 ceramide, C16:0 sphingomyelin, and C18:1 sphingomyelin were lower in liver transplantation (LT) recipients with than without AR. Comparisons with the results of LT patients with infection and cardiac transplant patients with cardiac allograft vasculopathy in humans and in mouse skin graft and hepatocyte transplant models suggested that the reduced C24 and C24:1 ceramides were specifically involved in AR. A ceramide synthase inhibitor, fumonisin B₁ exacerbated allogeneic immune responses in vitro and in vivo, and reduced tolerogenic dendritic cells (tDCs), while increased P3-like plasmacytoid DCs (pDCs) in the draining lymph nodes from allogeneic skin graft mice. The results of mixed lymphocyte reactions with ceranib-2, an inhibitor of ceramidase, and C24 ceramide also support that increasing ceramide concentrations could benefit transplant recipients with AR. The results suggest increasing ceramides as novel therapeutic target for AR, where reduced ceramides were associated with the changes in DC subsets, in particular tDCs.