• Proceedings of the Korean Nutrition Society Conference
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• 2003.05a
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• pp.184.1-184.1
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• 2003

• Analytical Science and Technology
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• v.16 no.1
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• pp.32-38
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• 2003

The rapid and sensitive determination method of sildenafil and its related compounds (Vardenafil, Homosildenafil, Tadanafil.) has been investigated using high performance thin layer choromatography (HPTLC). Optimizing separation conditions and simultaneous determination method of these compounds were studied. The calibration curves of those compounds at 254 nm was found to be linear in the range of $1.0{\sim}56.5{\mu}g/mL$, respectively. The detection limts (LOD) and quantification limits (LOQ) of these were found to be $0.8{\sim}1.8{\mu}g/mL$ and $1.0{\sim}2.3{\mu}g/mL$. The coefficient of variation (C.V.) were less than 2.5%. Finally, the present method was applied to determine sildenafil and its related substances in dietary supplement.

• Natural Product Sciences
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• v.22 no.3
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• pp.162-167
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• 2016

Peucedani Radix is the root of Angelica decursiva Franchet et Savatier (=Peucedanum decursivum Maximowicz) or Peucedanum praeruptorum Dunn in several Asian countries. The coumarins contained in Peucedani Radix were quantitatively analyzed using HPLC-DAD to develop a simultaneous determination for the quality control of A. decursiva and P. praeruptorum. For quantitative analysis, four major coumarins contained in these medicinal plants were assessed. Nodakenin (1), nodakenetin (2), praeruptorin A (3), and praeruptorin B (4) were separated with a Phenomenex Luna C18 column ($5{\mu}m$, $4.6{\times}250mm$) under the gradient conditions using distilled water with 0.1% phosphoric acid and acetonitrile with 0.1% phosphoric acid as the mobile phase, at a flow rate of 1.0 ml/min and a detection wavelength of 330 nm. This method was fully validated for linearity, accuracy, precision, recovery, and limit of detection and quantification. As a result, A. decursiva and P. praeruptorum were clearly classified by the quantification of four major coumarins in extracts. Also, the pattern recognition analysis based on HPLC indicates that all of the samples were largely clustered into two groups. Therefore, it is possible to distinguish between A. decursiva and P. praeruptorum and contribute to quality control.

• Analytical Science and Technology
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• v.15 no.3
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• pp.243-247
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• 2002

A rapid and simple determination of diazepam in intact diazepam tablets has been investigated using the near infrared spectroscopy(NIRS) combined with partial least squares regession. The separate calibration curves of 2 mg and 5 mg diazepam tablets were studied, as well as the linearity, concentration range and reproducibility of those calibration curves were evaluated. The correlation coefficients of calibration curves of 2 mg and 5 mg diazepam tablets are 0.9416 and 0.9159, respectively and the standard errors of calibration curves(SEC) are 0.018% and 0.032%, respectively.

• Mass Spectrometry Letters
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• v.13 no.3
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• pp.58-83
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• 2022

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL^-1; linearity (r²) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL^-1, linearity (r²) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

• Mass Spectrometry Letters
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• v.10 no.1
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• pp.18-26
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• 2019

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

• Toxicological Research
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• v.31 no.2
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• pp.137-149
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• 2015

Human hepatocytes, with complete hepatic metabolizing enzymes, transporters and cofactors, represent the gold standard for in vitro evaluation of drug metabolism, drug-drug interactions, and hepatotoxicity. Successful cryopreservation of human hepatocytes enables this experimental system to be used routinely. The use of human hepatocytes to evaluate two major adverse drug properties: drug-drug interactions and hepatotoxicity, are summarized in this review. The application of human hepatocytes in metabolism-based drug-drug interaction includes metabolite profiling, pathway identification, P450 inhibition, P450 induction, and uptake and efflux transporter inhibition. The application of human hepatocytes in toxicity evaluation includes in vitro hepatotoxicity and metabolism-based drug toxicity determination. A novel system, the Integrated Discrete Multiple Organ Co-culture (IdMOC) which allows the evaluation of nonhepatic toxicity in the presence of hepatic metabolism, is described.

• Journal of Food Hygiene and Safety
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• v.31 no.3
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• pp.186-193
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• 2016

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

• Proceedings of the PSK Conference
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• 2003.04a
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• pp.276.3-277
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• 2003

A simple, accurate GC analytical technique for the determination of phthalates. commonly used as plasticizers during the manufacturing process of PVC bags, in blood component preparations was developed and validated. The blood component preparations were extracted with n-hexane. The n-hexane layer was evaporated to dryness and the residue was dissolved in 1 $m\ell$ of n-hexane and analyzed by GC and GC/MS. (omitted)

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.