• Analytical Science and Technology
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• v.35 no.2
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• pp.60-68
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• 2022

In this study, we developed and validated a sensitive analytical method to quantify baphicacanthin A in mouse plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The standard calibration curves for baphicacanthin A ranged from 0.5 to 200 ng/mL and were linear, with an r² of 0.985. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. Besides, we investigated the pharmacokinetics of baphicacanthin A following its intravenous (5 mg/kg) and oral administration (30 mg/kg). Intravenously injected baphicacanthin A showed biphasic elimination kinetics with high clearance and volume of distribution values. Furthermore, baphicacanthin A showed a rapid absorption but low aqueous solubility (182.51±0.20 mg/mL), resulting in low plasma concentrations and low oral bioavailability (2.49 %). Thus, we successfully documented the pharmacokinetic properties of baphicacanthin A using this newly developed sensitive LC-MS/MS quantification method, which could be used in future lead optimization and biopharmaceutic studies.

• Korean Journal of Veterinary Service
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• v.45 no.3
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• pp.237-242
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• 2022

The simultaneous analysis of mycotoxins using LC-MS/MS, a food official analysis method, was applied with compound feed for pets with high consumer preferences. In this study, the linearity of all calibration curves showed good linearity of 0.99 or more. and both the accuracy (recovery rate) and precision (repeatability) criteria of the concentration range for each mycotoxin in the National Agricultural Products Quality Management Service's Validation and Verification Guidelines were met. And as a result of analyzing FAPAS QCM in the same way, it was assesed that the z-scores of Aflatoxin B₁, Ochratoxin A, Zearalenone, and Fumonisin B₁, were within ±2 range. This study showed that the application of the food official analysis method to compound feed for pets is suitable.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.47 no.4
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• pp.317-331
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• 2021

Essential oil is a volatile substance obtained by physically obtaining fragrant plant materials made by one single plant and plant species, and is widely used for cosmetics, fragrances, and aroma therapy due to its excellent preservation, sterilization, and antibacterial effects. When essential oil would undergo the extraction and concentration processes, the agricultural chemicals thereof would be extracted and concentrated only to be harmful to the human body. This study analyzes 320 residual agricultural chemicals concentrated in the essential oil, and to this end, LC-MS/MS and GC-MS/MS are used, while the freezing process is applied instead of the conventional refining process hexane, to improve the preprocessing method. As a result of analyzing the essential oil, such ingredients as chlorpyrifos, piperonyl butoxide and silafluofen have been detected in Basil oil and Clove leaf oil. Hence, it is perceived that the residual agricultural chemicals should continue to be monitored for the essential oil.

• Analytical Science and Technology
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• v.20 no.2
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• pp.138-146
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• 2007

A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

• Analytical Science and Technology
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• v.17 no.2
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• pp.117-129
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• 2004

Amitrole in environment, difficult to be analyzed by GC or GC/MS due to high polarity and low volatility, was analyzed by LC/ESI/MS in the study. Maximum peak intensity of amitrole in LC/MS/ESI mass spectrum is m/z 85 of protonated molecular ion $(M+H)^+$ with 30V of cone voltage at SIR mode. It was confirmed that ratios between main ion of amitrole, 85 of protonated molecular ion, and m/z 58 fragmented ion of amitrole, had increased corresponding with the increment of cone voltage from 20V to 70V. The isotope molecular weight of amitrole was $86([M+H])^+$ at LC/MS analysis and the mass spectrum ratio between 85 mass and 86 mass was not different by the change of concentration but similar to theoretical ratio(less than 10% standard deviation).The linearity of standard calibration curve under same condition with sample treatment method had $y=1.09354e^6X+26947.2$ and $r^2=0.99$. Recovery rates in water and soil samples were 77.64~83.44% and 71.11~79.44%, respectively. Reliability of the analysis was performed with 5 repeated measurements at each level of standard concentration and the result showed that relative standard deviation was less than 10%; therefore, the extraction and analysis method in the study suggested that it would be reliable to measure amitrole in water and soil media.

• Food Science of Animal Resources
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• v.35 no.4
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• pp.466-472
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• 2015

A rapid and simple analytical method, using liquid chromatography tandem mass spectrometry (LC-MS/MS), was developed to detect myo-inositol (MI) in infant formulas. For protein removal: acid hydrolysis and lipid removal through organic solvent extraction. The operating conditions for instrumental analysis were determined based on previously reported analogous methods that used LC-MS/MS. Quantitative analysis was used for the detection limit test, infant formula recovery test, and standard reference material (SRM) 1849a to verify the validity of our LC-MS/MS analytical method, which was developed to quantify MI. For validation, the results of our method were compared with the results of quantitative analyses of certified values. The test results showed that the limit of detection was 0.05 mg/L, the limit of quantitation was 0.17 mg/L, and the method detection limit was 17 mg/kg. The recovery test exhibited a recovery between 98.07-98.43% and a relative standard deviation between 1.93-2.74%. Therefore, the result values were good. Additionally, SRM 1849a was measured to have an MI content of 401.84 mg/kg and recovery of 98.25%, which is comparable to the median certified value of 409 mg/kg. From the aforementioned results, we judged that the instrumental analysis conditions and preparation method used in this study were valid. The rapid analytical method developed herein could be implemented in many laboratories that seek to save time and labor.

• Journal of the Korean Society of Tobacco Science
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• v.30 no.1
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• pp.33-38
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• 2008

This study was carried out to determine the analytical methods for heterocyclic amines(HAs) of the tobacco smoke by LC/MS/MS. HAs have been found in pyrolysate of protein and cooked food including protein, were known the Sugimura compound. HAs content of the smoke were known to exist very low ppb level. Especially, some of HAs are mutagenic and carcinogenic compounds. In according to IARC, the toxicity of N-heterocyclic amines classified IARC class 2A or 2B group. Precursors of these compounds are glutamic acid, protein and free amino acids including tryptophan, therefore, the precursors have been proved in cooked food continuously. This study was investigate multiple analysis methods for HAs and HAs contents of some commercial products. In this study, we used the linear type smoking machine for HAs analysis. At the ISO conditions, mainstream smoke was collected on cambridge filter pad, and then cambridge filter pad was extracted by 0.1% acetic acid. The extracted solution were passed cation exchange SPE cartridge to remove matrix, samples were analyzed using LC/MS/MS on MRM mode. From the result that optimized this methods, the correlation coefficient(R) of the individual compounds were good linearity over 0.999, recovery rate over 96% and the limit of detection were good values between 0.06 to 0.37 ng/mL, In addition, HAs content of some commercial products were in range of 0.02 to 43.8 ng/cig.

• Journal of Environmental Health Sciences
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• v.36 no.1
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• pp.44-51
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• 2010

This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.

• Analytical Science and Technology
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• v.24 no.4
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• pp.237-242
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• 2011

In this study, an analytical method was developed for residual metamizol in beef and pork using LC/MS/MS. 4-methylaminoantipyrin (MAA), the main metabolite of metamizol was targeted for analysis instead of its parent compound. MAA was simply extracted from meat by acetonitrile, purified and then analyzed by multiple reaction monitoring method (MRM). Standard addition method was used for calibration. The calibration curves showed the linearity of $r^2$ > 0.99 for both matrices included. The developed method was validated by six-time intra-lab tests and inter-lab tests with two other institutes. The validation of the whole procedure for beef showed the intra-lab accuracies of 78-102% (CV 5.5-9.1%) and the inter-lab accuracy of 98% (CV 14%); the intra-lab accuracies of 95-99% (CV 3.9-5.6%) and the inter-lab accuracy of 111% (CV 13%).

• Journal of Korean Society on Water Environment
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• v.25 no.5
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• pp.720-726
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• 2009

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.