• Mass Spectrometry Letters
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• 제5권3호
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• pp.84-88
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• 2014

Licoricidin isolated from Glycyrrhiza uralensis is known to have anticancer, anti-nephritic, anti-Helicobacter pylori, and antibacterial effects. In this study, a cocktail probe assay and liquid chromatography-tandem mass spectrometry (LC-MS/MS) were used to investigate the modulating effect of licoricidin on cytochrome P450 (CYP) enzymes in human liver microsomes. When licoricidin was incubated at $0-25{\mu}m$ with CYP probes for 60 min at $37^{\circ}C$, it showed potent inhibitory effects on CYP2B6-catalyzed bupropion hydroxylation and CYP2C9-catalyzed diclofenac 4'-hydroxylation with half maximal inhibitory concentration ($IC_{50}$) values of 3.4 and $4.0{\mu}m$, respectively. The inhibition mode of licoricidin was revealed as competitive, dose-dependent, and non-time-dependent, and following the pattern of Lineweaver-Burk plots. The inhibitory effect of licoricidin has been confirmed in human recombinant cDNA-expressed CYP2B6 and 2C9 with $IC_{50}$ values of 4.5 and $0.73{\mu}m$, respectively. In conclusion, this study has shown the potent inhibitory effect of licoricidin on CYP2B6 and CYP2C9 activity could be important for predicting potential herb-drug interactions with substrates that mainly undergo CYP2B- and CYP2C9-mediated metabolism.

• Mass Spectrometry Letters
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• 제12권2호
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• pp.53-58
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• 2021

Previous in vitro studies have demonstrated that ginsenoside Rc inhibits UGT1A9, but there are no available data to indicate that ginsenoside Rc inhibits UGT1A9 in vivo. The effect of single and repeated intravenous injection of ginsenoside Rc was evaluated on the pharmacokinetics of mycophenolic acid. After injection of ginsenoside Rc (5 mg/kg for one day or 3 mg/kg for five days), 2-mg mycophenolic acid was intravenously injected, and the pharmacokinetics of mycophenolic acid and mycophenolic acid-β-glucuronide were determined. Concentrations of mycophenolic acid and its metabolite from rat plasma were analyzed using a liquid chromatography-triple quadrupole mass spectrometry. Single or repeated pretreatment with ginsenoside Rc had no significant effects on the pharmacokinetics of mycophenolic acid (P > 0.05): The mean difference in maximum plasma concentration (C_max) and area under the concentration-time curve (AUC_inf) were within 0.83- and 0.62-fold, respectively, compared with those in the absence of the ginsenoside Rc. These results indicate that ginsenoside Rc has a negligible effect on the disposition of mycophenolic acid in vivo despite in vitro findings indicating that ginsenoside Rc is a selective UGT1A9 inhibitor. As a result, ginsenoside Rc has little possibility of interacting with drugs that are metabolized by UGT1A9, including mycophenolic acid.

• Mass Spectrometry Letters
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• 제12권1호
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• pp.16-20
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• 2021

We aimed to compare the content of ginsenosides and the pharmacokinetics after the oral administration of four different ginseng products at a dose of 1 g/kg in rats. The four different ginseng products were fresh ginseng extract, red ginseng extract, white ginseng extract, and saponin enriched white ginseng extract prepared from the radix of Panax ginseng C.A. Meyer. The ginsenoside concentrations in the ginseng product and the rat plasma samples were determined using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Eight or nine ginsenosides of the 15 tested ginsenosides were detected; however, the content and total ginsenosides varied depending on the preparation method. Moreover, the content of triglycosylated ginsenosides was higher than that of diglycosylated ginsenosides, and deglycosylated ginsenosides were not present in any preparation. After the single oral administrations of four different ginseng products in rats, only four ginsenosides, such as 20(S)-ginsenosides Rb1 (GRb1), GRb2, GRc, and GRd, were detected in the rat plasma samples among the 15 ginsenosides tested. The plasma concentrations of GRb1, GRb2, GRc, and GRd were different depends on the preparation method but pharmacokinetic features of the four ginseng products were similar. In conclusion, a good correlation between the area under the concentration curve and the content of GRb1, GRb2, and GRc, but not GRd, in the ginseng products was identified and it might be the result of their higher content and intestinal biotransformation of the ginseng product.

• Mass Spectrometry Letters
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• 제13권1호
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• pp.11-19
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• 2022

Although translational research is referred to clinical chemistry measures, correct weighting factors for linear and quadratic calibration curves with least-squares regression algorithm have not been carefully considered in bioanalytical assays yet. The objective of this study was to identify steroidogenic roles in preeclampsia and verify accuracy of quantitative results by comparing two different linear regression models with weighting factor of 1 and 1/x². A liquid chromatography-mass spectrometry (LC-MS)-based adrenal steroid assay was conducted to reveal metabolic signatures of preeclampsia in both serum and placenta samples obtained 15 preeclamptic patients and 17 age-matched control pregnant women (33.9 ± 4.2 vs. 32.8 ± 5.6 yr, respectively) at 34~36 gestational weeks. Percent biases in the unweighted model (w_i = 1) were inversely proportional to concentrations (-739.4 ~ 852.9%) while those of weighted regression (w_i = 1/x²) were < 18% for all variables. The optimized LC-MS combined with the weighted linear regression resulted in significantly increased maternal serum levels of pregnenolone, 21-deoxycortisol, and tetrahydrocortisone (P < 0.05 for all) in preeclampsia. Serum metabolic ratio of (tetrahydrocortisol + allo-tetrahydrocortisol) / tetrahydrocortisone indicating 11β-hydroxysteroid dehydrogenase type 2 was decreased (P < 0.005) in patients. In placenta, local concentrations of androstenedione were changed while its metabolic ratio to 17α-hydroxyprogesterone responsible for 17,20-lyase activity was significantly decreased in patients (P = 0.002). The current bioanalytical LC-MS assay with corrected weighting factor of 1/x² may provide reliable and accurate quantitative outcomes, suggesting altered steroidogenesis in preeclampsia patients at late gestational weeks in the third trimester.

• 분석과학
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• 제10권1호
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• pp.9-17
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• 1997

nitrophenol류는 미국 환경청에서 주요 priority 오염물질로 규정하고 있다. 물 중에 존재하는 nitrophenol류의 혼합물을 분석하기 위해 역상 액체크로마토그래피법에 대기압 화학이온화법을 연결한 질량분석기를 이용하였다. 추가적으로, 선택이온 검색법과 cone 전압차분해법(cone voltage fragmentation)을 이용하여 nitrophenol류의 확인에 있어서 감도와 선택성을 높였다. nitrophenol의 분해 형태는 충돌유발분해법인 MS/MS 기법으로 얻어진 분해 형태와 비교하였다.

• Journal of Applied Biological Chemistry
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• 제65권3호
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• pp.159-166
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• 2022

Epicoccum nigrum produces epipyrone A (orevactaene), a yellow polyketide pigment. Its biosynthetic gene cluster was previously characterized in E. nigrum KACC 40642. The YES liquid culture of this strain revealed high-level production of epicoccamide (EPC), with an identity that was determined using liquid chromatography-mass spectrometry analysis and molecular mass search using the SuperNatural database V2 webserver. The production of EPC was further confirmed by compound isolation and nuclear magnetic resonance spectroscopy. EPC is a highly reduced polyketide with tetramic acid and mannosyl moieties. The EPC structure guided us to localize the hypothetical EPC biosynthetic gene cluster (BGC) in E. nigrum ICMP 19927 genome sequence. The BGC contains genes encoding highly reducing (HR)-fungal polyketide synthase (fPKS)-nonribosomal peptide synthetase (NRPS), glycosyltransferase (GT), enoylreductase, cytochrome P450, and N-methyltrasnferase. Targeted inactivation of the HR-fPKS-NRPS and GT genes abolished EPC production, supporting the successful localization of EPC BGC. This study provides a platform to explore the hidden biological activities of EPC, a bolaamphiphilic compound.

• 한국건설순환자원학회논문집
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• 제8권1호
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• pp.129-133
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• 2020

우레아-포름알데히드(UF) 캡슐막의 마이크로캡슐 합성 공정에 있어서 반응 폐액에 포함된 포름알데히드의 잔류량을 GC-MS로 분석하였다. 포름알데히드의 반응에 영향을 주는 주된 인자로서 pH, 암모늄클로라이드 투입량, 온도의 3가지를 선정하고, 이 인자들이 반응 폐액 중의 포름알데히드 농도에 미치는 영향을 조사하였다. 실험 조건 중 암모늄클로라이드를 0.025g 투입한 경우에는 캡슐막 형성이 안 되거나 캡슐막이 약한 경향이 있어서 기본적으로 이 조건은 마이크로캡슐화에 부적절한 것으로 판단된다. 본 연구의 실험 조건에서 포름알데히드 잔류량이 최소화되는 마이크로캡슐화 조건은 70℃의 온도와 2.5의 pH에서 암모늄클로라이드를 0.050g 투입하는 조건임이 확인되었다. 본 연구의 결과는 보다 안전한 작업환경에서 마이크로캡슐화를 수행하는데 기여할 수 있을 것으로 기대된다.

• Journal of Microbiology and Biotechnology
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• 제26권7호
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• pp.1216-1223
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• 2016

The aim of this study was to isolate antioxidant peptides from an enzymatic hydrolysate of Spirulina platensis. A novel antioxidant peptide was obtained by ultrafiltration, gel filtration chromatography, and reverse-phase high-performance liquid chromatography, with the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay used to measure the antioxidant activity, and the sequence was determined to be Pro-Asn-Asn (343.15 Da) by electrospray ionization tandem mass spectrometry. This peptide was synthesized to confirm its antioxidant properties, and it exhibited 81.44 ± 0.43% DPPH scavenging activity at 100 μg/ml, which was similar to that of glutathione (82.63 ± 0.56%). Furthermore, the superoxide anion and hydroxyl free-radical scavenging activities and the SOD activity of the peptide were 47.84 ± 0.49%, 54.01 ± 0.82%, and 12.55 ± 0.75%, respectively, at 10 mg/ml. These results indicate that S. platensis is a good source of antioxidant peptides, and that its hydrolysate may have important applications in the pharmaceutical and food industries.

• 분석과학
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• 제28권1호
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• pp.1-7
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• 2015

4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), a tobacco specific nitrosamine found only in tobacco products. The ability to monitor biomarker concentrations is very important in understanding environmental tobacco smoke (ETS). In this study, an efficient and sensitive method for the analysis of NNK in dust was developed and validated using liquid chromatography tandem mass spectrometry. Dust was collected with filter paper soaked in methanol. The standard solution and dust sample were diluted with 100 mM ammonium acetate and extracted using dichloromethane. Our calibration curves ranged from 25 to $10^4pg/mL$. Excellent linearity was obtained with correlation coefficient values between 0.9996 and 1.0000. The limit of detection (LOD) was 5 pg/mL ($S/N{\geq}3$) and the retention time was 10 min. The limit of quantification (LOQ) was 25 pg/mL, and the acceptance criteria was the rate of 98-103% (80-120% at levels up to $3{\times}LOQ$). The coefficient of variations (CV) was 2.8%. Accuracies determined from dust samples spiked with four different levels of NNK racurves ranged that from 25 to 104 pg/mL. Excellent linearity was obtained between 92.1% and 114%. The precision of the method was acceptable (5% of CV). The recovery rates of the whole analytical procedure at low, medium, and high levels were 105.7-116.5% for NNK. The carry-over effects during LC-MS/MS analysis were not observed for NNK. This manuscript summarizes the scientific evidence on the use of markers to measure ETS.

• 한국약용작물학회지
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• 제25권3호
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• pp.146-151
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• 2017

Background: Rehmannia glutinosa is a perennial herb belonging to the family Scrophulariaceae. Its roots have been utilized as a traditional medicine. The aim of this study was to elucidate the basic information of the roots of the R. glutinosa cultivars and their utilization. Methods and Results: The roots of R. glutinosa cultivars were harvested in the end of March. The two iridoid glycosides, aucubin and catalpol, were analyzed by liquid chromatography/mass spectrometry (LC/MS), whereas ${\gamma}-aminobutyric$ acid (GABA) was analyzed by gas chromatography/mass spectrometry (GC/MS). The aucubin content was the highest in the Dakang cultivar, whereas no aucubin was detected in the five cultivars. All cultivars had more than 12 mg/g catalpol content, and the maximum catalpol content was found in Jihwang 1. The GABA content was the highest in Suwon 1, and it was 40 times more than that in the Yeongang cultivar. Conclusions: The highest aucubin, catapol and GABA contents were detected in the Dakang, Jihwang 1, and Suwon 1, cultivars respectively. This study provides the crucial information regarding the versatile utilization and pedigree selection of R. glutinosa cultivars.