• Bulletin of the Korean Chemical Society
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• v.35 no.4
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• pp.1133-1138
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• 2014

Ultrahigh performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI- MS/MS) provides a high-speed method to screen a large number of samples for small molecules with specific properties. In this study, UPLC-ESI-MS/MS with multiple reaction monitoring (MRM) was employed to screen urinary phospholipid (PL) content for biomarkers of prostate cancer. From lists of urinary PLs structurally identified using nanoflow LC-ESI-MS/MS, 52 PL species were selected for quantitative analysis in urine samples between 22 cancer-free urologic patients as controls and 45 prostate cancer patients. Statistical treatment of data by receiver operating characteristic (ROC) analysis yielded 14 PL species that differed significantly in relative concentrations (area under curve (AUC) > 0.8) between the two groups. Among PLs present at higher levels in prostate cancer urine, phosphatidylcholines (PCs) and phosphatidylinositols (PIs) constituted the major head group PLs (3 PCs and 7 PIs). For technical reasons, PL species of low abundance may be underrepresented in data from UPLC-ESI-MS/MS performed in MRM mode. However, the proposed method enables the rapid screening of large numbers of plasma or urine samples in the search for biomarkers of human disease.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.417-433
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• 2011

The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.

• YAKHAK HOEJI
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• v.40 no.2
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• pp.141-148
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• 1996

GC/MS analysis of 27 controlled pesticides in herbal drugs was studied. Selected ion monitoring(sim) technique was applied to increase the GC/MS sensitivity. Typical peaks in th e mass spectrum of each pesticides were selected as quantitation, comfirmation or alternate ion. Twenty seven pesticides were divided into five groups according to their retention time and the peaks for SIM were programmed accordingly. The combination of two ionization methods, electron impact(EI)-SIM-MS and negative ion chemical ionization(NCI)-SIM-MS, were well-fitted for the detection, confirmation and quantitation of multiclass residual pesticides in herbal drugs.

• Korean Journal of Food Science and Technology
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• v.46 no.5
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• pp.549-555
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• 2014

The geographical origin of commercial red ginseng concentrate was studied using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The ginsenoside content of domestic and Chinese red ginseng concentrates was determined. Four types of suspected origin samples could be selected this technique. The LC-MS/MS data were statistically analyzed on the basis of canonical function analysis and principal component analysis. Domestic and Chinese samples could be discriminated via canonical function analysis using posterior probability. In addition, the mixture ratio (Korean or Chinese origin) of the unknown origin specimen could be predicted based on the relationship between the mixing concentration of red ginseng concentrates and principal component 1.

• Korean Journal of Environmental Agriculture
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• v.39 no.2
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• pp.142-169
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• 2020

BACKGROUND: A new analytical method has been developed to determine 261 pesticide residues in herbal medicines. METHODS AND RESULTS: The extraction of pesticides was carried out by modified method of the Korea Food Standards Codex sample extraction and determination was performed using GC-MS/MS and LC-MS/MS. During the pre-treatment process of the test method, Solid-liquid separation was changed to centrifugation. The method was validated by the precision and accuracy results. 261 pesticides spiked at three level 20, 50, 100 ug/kg in herbal medicines. The limit of quantification of method were 4-40 ug/kg for GC-MS/MS and 2-45 ug/kg for LC-MS/MS, respectively. Among the pesticides analysed by GC-MS/MS and LC-MS/MS, 244 pesticides (94% of total number) in chinese matrimony vine and 224 pesticides (86% of total number) in korean angelica root and 231 pesticides (89% of total number) in jujube and 214 (82% of total number) in cnidium showed recoveries in the range of 70-120% with RSD⪯20%. CONCLUSION: These results indicated that GC-MS/MS and LC-MS/MS analysis with the sample extraction in this study can be applied to multi-residue analysis of pesticides in herbal medicines.

• Food Science of Animal Resources
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• v.34 no.5
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• pp.656-664
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• 2014

The purpose of this study was to analyze myosin heavy chain (MHC) isoforms in bovine longissimus thoracis (LT) muscle by liquid chromatography (LC) and mass spectrometry (MS). LT muscles taken from Hanwoo (Korean native cattle) steer (n=3) used to separate myosin bands by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The peptide queries were obtained from the myosin bands by LC-MS/MS analysis following in-gel digestion with trypsin. A total of 33 and 43 queries were identified as common and unique peptides, respectively, of MHC isoforms (individual ions scores >43 indicate identity or extensive homology, p<0.05). MHC-1 (IIx), -2 (IIa), -4 (IIb), and -7 (slow/I) were identified based on the Mowse score (5118, 3951, 2526, and 2541 for MHC-1, -2, -4, and -7, respectively). However, more analysis is needed to confirm the expression of MHC-4 in bovine LT muscle because any query identified as a unique peptide of MHC-4 was not found. The queries that were identified as unique peptides could be used as peptide markers to confirm MHC-1 (14 queries), -2 (8 queries), and -7 (21 queries) in bovine LT muscle; no query identified as a unique peptide of MHC-4 was found. LC-MS/MS analysis is a useful approach to study MHC isoforms at the protein level.

• Korean Journal of Pharmacognosy
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• v.51 no.3
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• pp.207-216
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• 2020

The analysis method for qualitative analysis of the screening method that can be performed prior to the quantitative analysis of individual pesticide was reviewed in order to meet the safety standards that are being strengthened in the field of pesticide residue testing of herbal medicines. Among the residual pesticides presented in the Korean Pharmacopoeia, 56 pesticides, excluding 15 pesticides that need to be individually analyzed, were selected for analysis using QuEChERS preprocessing and GC-MS/MS, which are used in the existing agricultural products field. For each pesticide, the detection limit level of 0.001-0.005 mg/kg and the quantitative limit level of 0.002-0.017 mg/kg were confirmed. In the recovery test in which the standard was treated at a concentration of 0.02 mg/kg, it was confirmed that the proportion of pesticides satisfying the recovery of 70-120% was 85.7-96.4% for each herbal medicine, so it was confirmed that it was a level that could be reviewed by the screening method.

• 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.

• Journal of the Korean Society of Tobacco Science
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• v.29 no.2
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• pp.132-139
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• 2007

This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

• YAKHAK HOEJI
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• v.60 no.1
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• pp.15-20
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• 2016

Globotriaosylsphingosine (lyso Gb3) is considered as one of the biomarkers for Fabry disease. A rapid and simple UPLC-MS/MS method was developed for the determination of reliable biomarker, lyso Gb3. Total analytical procedure takes only 15 min including sample preparation and MS/MS analysis. Limit of detection was 0.85 ng/ml (S/N=3). The calibration curve was linear over the range of 2.0~400.0 ng/ml ($R^2=0.9999$). Inter-day and intra-day assay accuracy were 93.4~100.6% (RSD, 0.6~6.0%) and 97.5~100.7% (RSD, 3.6~5.2%). Absolute recoveries of 97.6~98.6 showed excellence of a new analytical method. The method was applied to human and mice urines, proved the suitability for the quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.