• Title/Summary/Keyword: liquid chromatography mass spectrometry

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Characteristics of PAH Occurrence during Meat Cooking (육류가공식품의 조리방법에 따른 PAHs 발생 특성에 관한 연구)

  • Lee, Byung ho;An, Yu Jin;Park, Dong Yun;Byun, Gi Young;Kim, Kyoung Dong;Lee, Mi Lim;Seo, Jung Bum;Park, Eun Young;Park, Heung Jai
    • Journal of Environmental Science International
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    • v.25 no.11
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    • pp.1459-1466
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    • 2016
  • In this study, the concentrations of polycyclic aromatic hydrocarbons (PAHs) were investigated in meat process food and for cooking methods (pan-frying and charcoal fire). The methodology involved liquid-liquid extraction, silica gel cartridge clean-up and determination by gas chromatography/mass spectrometry (GC/MS). The recovery of 17 PAHs spiked into these samples ranged from 66.6 % to 98.0% and the coefficient of variation was less than 10%, but that of dibenz(a,h)anthracene was 16.39%. The mean concentration of total PAHs in processed samples was ND~7.2 ng/g, whereas that pan-fried and charcoal-fired samples were ND~22.1 ng/g and, 12.7~367.8 ng/g, respectively. Therefore, the concentrations of total PAHs in cooked samples were higher than in original samples and charcoal-fired samples had the highest total PAH levels.

Bisphenol-A Concentrations from Leiomyoma Patients by LC/MS

  • Han, Myoung-Seok;Byun, Jae-Chun;Park, Ji-Eun;Kim, Ji-Young;Chung, Jin-Yong;Kim, Jong-Min
    • Toxicological Research
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    • v.27 no.1
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    • pp.49-52
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    • 2011
  • The aim of this study is to investigate how many leiomyoma patients are exposed to bisphenol-A (BPA), an endocrine disruptor, and whether the serum concentration of BPA is related to leiomyoma growth. Initially, 128 patients were divided into one control and three leiomyoma groups (mild, moderate and severe) according to the size of the leiomyomas. Serum BPA concentrations were measured by liquid chromatography and mass spectrometry (LC/MS). Nearly two-thirds of leiomyoma patients were exposed to BPA and the range of BPA was from non-detection to 2.603 ng/ml. The mean BPA concentrations in the groups were $1.015{\pm}0.775\;ng/ml$ (control), $0.774{\pm}0.834\;ng/ml$ (mild), $1.261{\pm}0.797\;ng/ml$ (moderate) and $1.244{\pm}0.860\;ng/ml$ (severe) (p = 0.158). After recombination into two group, Group 1 (control plus mild) vs. Group 2 (moderate plus severe), higher level was found in Group 2 even with no statistical significance (p = 0.06). In conclusion, about two-thirds of leiomyoma patients were exposed to BPA, but it may not have growth promoting effect on leiomyoma.

Bioequivalence and Pharmacokinetic study of Gabapentin 300mg Capsules using Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS) in Volunteers (LC/MS/MS를 이용한 가바펜틴 300 mg 캡슐의 성인 지원자에 대한 생물학적 동등성 및 약물동태 연구)

  • Jeong, Ji-Hoon;Kwon, Jun-Tack;Yun, Hwi-Yeol;Kang, Won-Ku;Kwon, Kwang-Il
    • Korean Journal of Clinical Pharmacy
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    • v.16 no.1
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    • pp.63-68
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    • 2006
  • Gabapentin, 1-(aminomethyl-1-cyclohexyl)acetic acid, is anew antiepileptic drug related to ${\gamma}-aminobutyric$ acid(GABA) currently being introduced in therapy worldwide. The bioavailability and pharmacokinetics of gabapentin capsules were examined in 22 volunteers who received a single oral dose in the fasting state by randomized balanced $2{\times}2$ crossover design. After dosing, blood samples were collected for a period of 24 hours and analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS). Time course of plasma gabapentin concentration was analyzed with non-compartmental and compartmental approaches. $WinNonlin^{(R)}$, the kinetic computer program, was used for compartmental analysis. One compartment model with first-order input, first-order output with no lag time and weighting by $1/(predieted\;y)^2$ was chosen as the most appropriate pharmacokinetic model for the volunteers. The major pharmacokinetic parameters $(AUC_{0-24hr},\;AUC_{inf},\;C_{max}\;and\;T_{max})$ and other parameters $(K_a,\;K_{el},\;V_d/F\;and\;Cl/F)$ of $Gapentin^{TM}$ (test drug) and $Neurontin^{TM}$ (reference drug) were estimated by non-compartmental analysis and compartmental analysis. The 90% confidence intervals of mean difference of logarithmic transformed $AUC_{0-24hr}\;and\;C_{max}$ were $log(0.9106){\sim}log(1.l254)\;and\;log(0.8521){\sim}log(1.0505)$, respectively. It shows that the bioavailability of the test drug is equivalent with that of the reference drug. There was no statistically significant difference between the two drugs in all pharmacokinetic parameters.

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Deastringent Peel Extracts of Persimmon (Diospyros kaki Thunb. cv. Cheongdo-Bansi) Protect Neuronal PC-12 and SH-SY5Y Cells against Oxidative Stress

  • Jeong, Da-Wool;Cho, Chi Heung;Lee, Jong Suk;Lee, Seung Hwan;Kim, Taewan;Kim, Dae-Ok
    • Journal of Microbiology and Biotechnology
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    • v.28 no.7
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    • pp.1094-1104
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    • 2018
  • The peel of astringent persimmon (Diospyros kaki Thunb. cv. Cheongdo-Bansi) is a by-product of dried persimmon (gotgam). We investigated if deastringent peel extracts of persimmon cv. Cheongdo-Bansi had antioxidative and neuroprotective properties. Two different extracts were prepared: thermally and nonthermally treated persimmon peel extracts (TPE and NTPE, respectively). Both TPE and NTPE were fractionated sequentially in n-hexane, chloroform, ethyl acetate, n-butanol, and water. The TPE and NTPE ethyl acetate fractions had the highest total phenolic and flavonoid contents as well as antioxidant capacities among all the fractions. Pretreatment of neuronal PC-12 and SH-SY5Y cells with the TPE and NTPE ethyl acetate fractions increased cell viability after exposure to oxidative stress. The ethyl acetate fraction of TPE attenuated oxidative stress inside both PC-12 and SH-SY5Y cells more effectively than that of NTPE. Furthermore, the TPE and NTPE ethyl acetate fractions inhibited acetylcholinesterase and butyrylcholinesterase. Analysis of ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry results revealed gallic acid, kaempferol, kaempferol-3-O-galactoside, kaempferol-3-O-glucoside, quercetin, quercetin3-O-galactoside, quercetin-3-O-galactoside-2'-O-gallate, and quercetin-3-O-glucoside as the major phenolics of the TPE and NTPE ethyl acetate fractions. Taken together, these results suggest that the ethyl acetate fraction of deastringent persimmon peel is rich in antioxidants and has potential as a functional food to reduce oxidative stress.

Measurement of the Rate of Protein Synthesis in Chickens by HPLC/MS

  • Seo, S.S.;Coon, C.
    • Korean Journal of Poultry Science
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    • v.31 no.3
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    • pp.137-143
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    • 2004
  • The fractional synthesis rates(FSR) were measured with 2l-wk and 3l-wk-old broiler breeder pullets and hens to investigate the effect of sexual maturity on FSR. The FSR were obtained from chicken tissues and blood samples using High-Performance Liquid Chromatography/Mass Spectrometry(HPLC/MS). A L-l-13C, 15N -leucine saline solution was infused by bolus injection as a tracer into broiler breeder pullets in the experiment. A rapid HPLC/MS method was developed to measure the isotopic enrichments of leucine in plasma, tissue samples, and eggs. The enrichments of stable isotope leucine incorporated into protein and the enrichments of the stable isotope free leucine were measured in liver, breast muscle and blood samples. Two sets of experiments were conducted. In experiment one, 2l-wk-old, sexually immature broiler breeder pullets were divided into groups of three and blood samples were collected at 20 or 30 min intervals until 1.5 h from initial injection. The pullets were sacrificed in groups of three at varying time intervals for 7 h after injection. The liver, breast muscle and blood samples were removed for analysis. The FSR were estimated to be 8.7l%/day for liver, 4.06%/day for breast muscle, and 5.08%/day for blood samples in 30 minutes after injection from the enrichment ratios. In experiment two, sexually matured 3l-wk-old broiler breeder hens were assorted into groups of three and blood samples were obtained at 20 or 30 min intervals for 2 h. The FSR for blood samples were determined. The broiler breeder hens were sacrificed in groups of three at various time intervals until 7 h after injection and liver, breast muscle and blood samples were removed for analysis. The FSR were calculated to be 5.96%/day for liver. Eggs were collected from five chickens daily for 10 days after large bolus injection. The average of total enrichments of stable isotope in egg albumin was increased by 0.064% at 4 days after injection and was back to normal in 7 days.

Analysis of antibiotic residues in milk from healthy dairy cows treated with bovine mastitis ointment using ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry

  • Park, Eun-Kee;Ryu, Yong-Jae;Cha, Chun-Nam;Yoo, Chang-Yeul;Kim, Suk;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.56 no.4
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    • pp.233-239
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    • 2016
  • This study was conducted to analyze penicillin G (PEG), streptomycin (STR) and neomycin (NEO) residues in milk of healthy lactating cows. Milk samples were collected from all four quarters of 12 dairy cows 2−7 days after intramammary infusions of an ointment containing PEG, STR and NEO once (n = 4; group I) or twice (n = 4, group II) daily. Ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry was used to determine the antibiotic residues in the samples. The correlation coefficient ($r^2$) of the calibration curves for all antibiotics was > 0.999 and the limits of detection and quantification were $0.002-0.005{\mu}g/mL$ and $0.007-0.02{\mu}g/mL$, respectively. Recovery rates were ranged from 75.5 to 92.3%. In group I, PEG, STR and NEO residues were detected in milk at 2, 3 and 2 days post-treatment, respectively, which were below the maximum residue limit (MRL). In group II, PEG, STR and NEO residues were detected in milk at 2, 3 and 3 days post-treatment, respectively, which were bellow the MRL. These results suggest that a 3-day for milk withdrawal period after the ointment treatment might be sufficient for reduction of the antibiotic residues below the MRL.

Quantitative Analysis of the Marker Constituents in Yongdamsagan-Tang using Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (LC-ESI-MS/MS를 이용한 용담사간탕의 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.48 no.4
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    • pp.320-328
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    • 2017
  • Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

Quantification of the 25 Components in Onkyung-Tang by Ultra Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (UPLC-ESI-MS/MS를 이용한 온경탕 중 25종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.47 no.1
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    • pp.92-101
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    • 2016
  • In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

Analysis of Acrylamide in Mainstream Cigarette Smoke and Effects of Total Nitrogen and Reducing Sugars on Acrylamide Content

  • Kim, Ick-Joong;Lee, John-Tae;Min, Hye-Jeong;Kim, Hyo-Keun;Hwang, Keun-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.140-145
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    • 2007
  • Acrylamide has been found in many foods. Acrylamide in foodstuffs were analyzed by a GC/MS after bromination of acrylamide or by a LC/MS for underivatized acylamide. Time consuming and laborious clean up procedures is applied for the purification of the extract, in these methods. In this study, a simple and fast method without clean up step for the analysis of acrylamide in mainstream cigarette smoke was developed by using liquid chromatography-tandem mass spectrometry (LC/MS/MS) and the effects of tobacco leaf constituents on acrylamide content was observed. The analysis of acrylamide in mainstream cigarette smoke started to collect TPM (total particulate matter) from smoking and to extract by 0.1 % acetic acid solution and then to detect by liquid chromatography tandem mass spectrometry using electrospray in the positive mode. The recovery of acrylamide in 2R4F reference cigarette was 98 % and the reproducibility was 2.5 % and the limit of detection was 1.6 ng/mL. Reducing sugars and amino acids are considered to be main precursors of acrylamide in foodstuffs. Cut tobacco contain substantial amounts of reducing sugars and amino acid which may be explained the occurrence of acrylamide in mainstream cigarette smoke. The effects of reducing sugars and total nitrogen studied in an experiment with a various tobacco types. This result indicated that reducing sugars are not limiting factor for acrylamide formation, but the level of acrylamide in cigarette smoke was significantly correlated with the total nitrogen contents.

Analysis of polyphenolic metabolites from Artemisia gmelinii Weber ex Stechm. and regional comparison in Korea

  • Park, Mi Hyeon;Kim, Doo-Young;Jang, Hyun-Jae;Jo, Yang Hee;Jeong, Jin Tae;Lee, Dae Young;Baek, Nam-In;Ryu, Hyung Won;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
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    • v.62 no.4
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    • pp.433-439
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    • 2019
  • Artemisia species are widely used as food ingredients and raw material in traditional medicine. However, to date, the secondary metabolites of Artemisia gmelinii Weber ex Stechm. have not been sufficiently investigated. The secondary metabolites of A. gmelinii, which was collected from representative regions in Chungbuk, Gangwon, and Gyeongbuk, were analyzed using ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTof MS) combined with an unsupervised principal component analysis (PCA) multivariate analysis. In the loading scatter plot of PCA, significant changes in metabolites were observed between the regions, ten metabolites (3: 5-O-caffeoylquinic acid, 4: 4-O-caffeoylquinic acid, 8: trans-melilotoside, 12: quercetin 3-O-hexoside, 15: 3,4-O-dicaffeoylquinic acid, 17: 3,5-O-dicaffeoylquinic acid, 18: 4,5-O-dicaffeoylquinic acid, 19: syringaldehyde, 20: caffeoylquinic acid derivative, and 23: icariside II) were evaluated as key markers among twenty-five identified metabolites. Interestingly, the contents of the identified marker significantly differed between the three groups. This is the first study to report the presence of marker metabolites and their correlating geographical cultivation in A. gmelinii.