• Mass Spectrometry Letters
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• v.2 no.2
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• pp.37-40
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• 2011

Saccharin is a commonly used artificial sweetener in foodstuffs. However, for its carcinogenic dispute, it has been regulated by government bodies. In this study, isotope dilution mass spectrometry (ID-MS) was introduced for the accurate quantification of saccharin. To employ ID-LC/MS, we obtained its isotope analogue, $^{13}C_1$-sodium saccharin, by customized synthesis. Samples were spiked with $^{13}C_1$-sodium saccharin and analyzed with LC/MS in negative mode. Chromatographic conditions were optimized for the adequate chromatographic retention and separation of saccharin with a $C_{18}$ column. MS was operated with electrospray ionization by the selected ion monitoring (SIM) mode of $[M-H]^-$ for saccharin (m/z 182) and $[M-Na]^-$ for its isotope analogue (m/z 183). To validate the ID-LC/MS method for accurate measurement, we prepared a batch of a candidate material by sortifying quasi-tea-drinks with saccharin and analyzed samples gravimetrically fortified in various levels of concentration. The repeatability and reproducibility of this method was tested by analyzing the reference material. Result show that ID-LC/MS is a reliable method for the quantitative analysis of saccharin.

• Bulletin of the Korean Chemical Society
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• v.28 no.5
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• pp.745-750
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• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of folic acid in infant milk formula. Sample was spiked with 13C5-folic acid and then extracted with phosphate buffer (pH 6) solution. The extract was further cleaned up by deproteinization followed by a C18 solid-phase extraction cartridge. The extract was analyzed by using LC/ ESI/MS/MS with selectively monitoring the collisionally induced dissociation channels of m/z 442 → m/z 295 and m/z 447 → m/z 295, which are the neutral glutamyl loss from the [M+H]+ ions of folic acid and 13C5-folic acid, respectively. LC/MS/MS chromatograms showed substantially reduced background from chemical noises compared to LC/MS chromatograms. Repeatability and reproducibility studies showed that the LC/MS/ MS method is a reliable and reproducible method which can provide less than 1.5 relative percentage of method precision.

• Analytical Science and Technology
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• v.28 no.5
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• pp.317-322
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• 2015

Simultaneous analytical method has developed for the determination of anion biocides in soil by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chlorite and chlorate in soil were extracted with pure water, and cyanuric acid and sodium dodecylbenzenesulfonate (Na-DBS) were extracted with mobile phase (0.25 mM ammonium formate in 20 mM formic acid : acetonitrile (1:1)). The extract was injected into the LC-MS/MS system after filtration. The method detection limits in this study were 0.04 mg/kg for chlorite, 0.04 mg/kg for chlorate, 0.27 mg/kg for cyanuric acid, and 0.05 mg/kg for Na-DBS, respectively. The method was applied to the analysis of 50 soil samples collected from 40 sites sprayed with biocides and 10 background sites. As a result, anion biocides were not detected in all sites.

• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.46-54
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• 2022

Known for its effectiveness in weight loss and diabetes prevention, Gymnema sylvestre products can be found in the US, Japanese, and Indian markets. However, the recommended dosage or safety of these products has not yet been proven. Therefore, development of an analytical method for detecting the content of Gymnema sylvestre in food products is required. Accordingly, this study proposes an analysis method that can examine Gymnema sylvestre in food using LC-ESI-MS/MS and KASP (Kompetitive Allele-Specific PCR) markers. In LC-ESI-MS/MS, a simultaneous analysis method for gymnemic acid and deacylgymnemic acid was optimized using negative ionization mode, and its validation test was completed for solid and liquid samples. In addition, KASP markers were prepared by finding the specific SNP of G. sylvestre in ITS2 and matK through DNA barcodes. The two KASP markers returned positive FAM fluorescence result when combined with G. sylvestre, and this aspect was confirmed in raw G. sylvestre as well. The applicability of the method was tested on 21 different food and healthy functional products containing G. sylvestre purchased on the internet. As a result, although there was a difference in the ratios of gymnemic acid and deacylgymnemic acid in LC-ESI-MS/MS, the index component was detected in all 21 products samples. In the KASP analysis, 9 products returned positive FAM result, and the rest of the products were found to be containing G. sylvestre extract. This study is the first study to use the dual system of LC-ESI-MS/MS and KASP for the analysis of G. sylvestre. The study has confirmed that these two methods are applicable to the examine G. sylvestre content in food products.

• Korean Journal of Veterinary Service
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• v.28 no.1
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• pp.81-89
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• 2005

Recently, mass spectrometry coupled with liquid chromatography (LC/MS) has been a preferred technique for determination of organic compounds in complex matrixes. LC/MS provides a high degree sensitivity and specificity of the compounds of interest. The purpose of this study was to confirm analytical method of residual 6 benzimidazoles (thiabendazole, oxfendazole, mebendazole, albendazole, flubendazole and fenbendazole) in meat by LC/MS. Benzimidazoles were analyzed by LC/MS on XTerra $C_{18}$ column with 0.01% trifluoroacetic acid-acetonitrile (TFA) in a gradient mode as mobile phase, and that were identified by electrospray ionization with selected ion recording mode at 150-350 amu mass range. Residual benzimidazoles were extracted from tissue with ethylacetate, and elute benzimidazoles with $50\%$ acetonitrile. In the LC/MS analysis of benzimidazoles, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via $[M+H]^+$ and Fragment ions. A spectrum of benzimidazoles was showed from all 6 benzimidazoles

• Analytical Science and Technology
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• v.20 no.3
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• pp.198-203
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• 2007

The analysis method of 3-Monochloropropane-1,2-diol (3-MCPD) compound in water was developed using liquid chromatography with mass spectrometric detection. Aqueous solution was controlled in strong basic condition with sodium hydroxide, and then $25{\mu}L$ of benzoyl chloride was added to the solution for the derivatization of 3-MCPD. The derivative was extracted using pentane and analyzed by the selected ion monitoring (SIM) method of LC-MS. The results of analyses showed that the calibration curves was in the range of 1.0 to $100{\mu}g/mL$ with a good linearity (correlation coefficient of $r^2=0.992$) and limit of detection was below $0.01{\mu}g/mL$. The recoveries of this analysis method by LC-MS were 92.3-98.0 %.

• Analytical Science and Technology
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• v.15 no.6
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• pp.574-579
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• 2002

A sensitive and easy high performance liquid chromatograph (HPLC) / electrospray ionization (ESI)-mass spectrometric (MS) method has been developed for the quantitative and qualitative analyses of acarbose and its metabolites. After plasma samples were simply filtered with a syringe filter, the filtered plasma was analyzed by LC/MS. The standard calibration curve for acarbose was linear ($r^2=0.9963$) over the concentration range $0.1{\sim}10{\mu}g/m{\ell}$ in plasma. The metabolite component-I and II, which were metabolized by the ${\alpha}$-amylase and ${\beta}$-amylase, were found also by in vitro incubation. The developed method can be utilized to study acarbose and the other carbohydrates.

• Proceedings of the Korean Society for Bioinformatics Conference
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• 2004.11a
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• pp.167-177
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• 2004

본 논문에서는 LC/MS 데이터로부터 동위 원소 패턴(isotope pattern)을 찾는 새로운 방법을 제시하고자 한다. 기존의 분석 방법에서는 LC/MS 데이터를 1차원적으로 분석하고 있기 때문에 2차원에서 적용할 수 있는 알고리즘을 적용하기가 어렵다. LC/MS 데이터를 2차원 영상으로 가시화해 본 결과, 하나의 동위 원소 패턴에 속하는 단일 동위 원소 피크(single isotope peak)는 모양, 크기와 같은 2차원 형태적 특징들도 유사함을 알 수 있다. 따라서, 기존의 방법들이 질량 스펙트럼과 같은 1차원 신호를 분석하는 것에 중점을 둔 것에 비해, 본 논문에서는 LC/MS 데이터를 2차원 신호 즉, 영상(image)으로 간주하고 영상 처리 방법과 객체 인식 방법을 적용하였다. 실험 결과 같은 동위 원소 패턴에 속하는 각각의 단일 동위원소 피크들 사이에 peak maxima position 뿐만 아니라 skewness, variance등도 유사였으며 이러한 유사도를 기반으로 동위 원소 패턴을 찾을 수 있었다.

• Korean Journal of Veterinary Service
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• v.25 no.3
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• pp.221-227
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• 2002

This study was carried out to confirm analytical method of residual macrolides in livestock products by LC/MS. 1. Macrolides were analyzed by LC/MS on XTerra C$\sub$18/ column with 0.1% TFA(trifluoroacetic acid)-methanol in a gradient mode as mobile phase, and that were identified by positive chemical ionization with selective ion monitoring at 50～1000 mass range. 2. Residual macrolides were extracted from tissue with acetonitrile, and the extract is purified with a Sep-pak C$\sub$18/ cartridge, and elute macrolides with 0.1M methanolic ammonium acetate. 3. The procedure confirms the presence of each macrolide at 50$\mu\textrm{g}$/kg in spiked sample.

• Proceedings of the Korean Society for Bioinformatics Conference
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• 2004.11a
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• pp.296-306
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• 2004

LC/MS를 이용하여 펩타이드 혹은 단백질 같은 물질을 분석하는 실험이 급격히 늘어남에 따라 LC/MS 데이터를 자동으로 처리하는 기술에 대한 요구가 커지고 있다. 이러한 LC/MS 데이터의 자동 분석 기술에 대한 연구는 현재 활발히 진행되어 왔고, 이를 직접 구현한 여러 상용 소프트웨어들이 개발되어 있는 상태이다. LC/MS 데이터는 noise 제거, background 데이터 제거, deconvolution 알고리즘을 적용한 분자량(molecular weight) 할당 등의 작업을 거쳐 분석하게 된다. 이러한 과정을 거쳐 얻어진 분자량에 대한 데이터가 올바른 값인지 검증하는 작업이 필요하다. 본 논문에서는 이러한 검증 작업과 관련하여 Peak Clustering and Fitting(이하 PC&F)에 대한 알고리즘을 제안한다. PC&F은 peak 데이터들이 지니고 있는 속성에 대한 Mahalanobis distance를 이용하여 peak 데이터를 각 retention time에 따라 clustering 분석을 하는 작업이다. 본 논문에서 제안하는 PC&F 알고리즘을 Microsoft Visual C++ 6.0 MFC 환경에서 직접 개발한 소프트웨어(PeakClusterFitLCMS)로 실험하였다. 실험결과 PC&F 작업을 통해 동일한 구성물질로부터 발생한 peak 데이터를 모아서 보다 신뢰할 수 있는 분자량을 구할 수 있었고, 구성물질에 의해 발생되지 않은 noise peak 데이터를 찾아 제거시킬 수 있음을 확인할 수 있었다.