• Title/Summary/Keyword: LC-MS-MS

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Determination of 11 Illicit Compounds in Dietary Supplements Using High-Performance Liquid Chromatography and Liquid Chromatography-Tandem Mass Spectrometry

  • Shin, Dasom;Kang, Hui-Seung;Kim, Hyung-soo;Moon, Guiim
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.326-333
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    • 2020
  • In this work, we developed an analytical method for determining 11 illicit compounds in dietary supplements using high-performance liquid chromatography and liquid chromatography-tandem mass spectrometry. Eleven target compounds, including those meant for weight loss (7-keto-dihydroepiandrosterone, buformin, metformin, phenformin, salbutamol, and tolbutamide), sexual enhancement (dihydroepiandrosterone), and relaxation (asarone, kavain, magnoflorine, and picamilon) were screened and confirmed in dietary supplements. Method validation was performed by evaluating the selectivity, linearity, limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was > 0.993 for all analytes. The LOQs were ranged in 2.1-9.9 ㎍/mL (HPLC-DAD) and 0.002-0.008 ㎍/mL (LC-MS/MS). The accuracies (expressed as recovery) were 90.0-106% (HPLC-DAD) and 83.0-114% (LC-MS/MS). The precision (expressed as the relative standard deviation) was below 10% using HPLC and LC-MS/MS. The proposed method can be used for the surveillance of illicit compounds in dietary supplements.

Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

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 $548.13{\mu}g/g$.

Biotransformation of Valdecoxib by Microbial Cultures

  • Srisailam, K.;Veeresham, C.
    • Journal of Microbiology and Biotechnology
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    • v.20 no.4
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    • pp.809-816
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    • 2010
  • Microbial biotransformations can be used to predict mammalian drug metabolism. The present investigation deals with microbial biotransformation of valdecoxib using microbial cultures. Thirty-nine bacterial, fungal, and yeast cultures were used to elucidate the biotransformation pathway of valdecoxib. A number of microorganisms metabolized valdecoxib to various levels to yield nine metabolites, which were identified by HPLC-DAD and LC-MS-MS analyses. HPLC analysis of biotransformed products indicated that a majority of the metabolites are more polar than the substrate valdecoxib. Basing on LC-MS-MS analysis, the major metabolite was identified as a hydroxymethyl metabolite of valdecoxib, whereas the remaining metabolites were produced by carboxylation, demethylation, ring hydroxylation, N-acetylation, or a combination of these reactions. The hydroxymethyl and carboxylic acid metabolites were known to be produced in metabolism by mammals. From the results, it can be concluded that microbial cultures, particularly fungi, can be used to predict mammalian drug metabolism.

Comparison of Concentration of Urinary Metabolites of PAHs from Smokers and Nonsmokers (흡연자와 비흡연자의 소변 중 다환방향족탄화수소(PAHs) 대사체 농도 비교)

  • Kho, Young-Lim;Lee, Eun-Hee
    • Journal of Environmental Health Sciences
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    • v.37 no.6
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    • pp.474-481
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    • 2011
  • This study investigated urinary metabolites of polycyclic aromatic hydrocarbons (PAHs) in the urine of smokers and non-smokers by liquid chromatography triple quordrupole tandem mass spectroscopy (LC/MS/MS). Compounds analyzed for urinary biomarkers of PAHs were five mono-hydroxylated PAHs metabolites; 1-naphthol, 2-naphthol, 1-hydroxypyrene(1-OHP), 3-phenanthrol, 2-fluorenol. Urine samples were pretreated by enzymatic hydrolysis and solid phase extraction method. Smokers were composed of 17 men and five women; non-smokers 17 men and 16 women. Smoking increased urinary concentrations of five PAHs metabolites significantly higher than those of nonsmokers. Statistically significant correlations among the five PAHs metabolites were shown. The results suggest that LC/MS/MS technology should be useful in the environmental health discipline.

Mass Spectrometric Analysis for Discrimination of Diastereoisomers

  • Manshoor, Nurhuda;Weber, Jean-Fré
    • Mass Spectrometry Letters
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    • v.6 no.4
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    • pp.99-104
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    • 2015
  • A liquid chromatography mass spectrometry (LC-MS) system was used to identify and distinguish oligostilbene diastereoisomers. A polyphenolic extract from Neobalanocarpus heimii known to be rich in oligostilbenes of various degrees of condensation was used as test material. Fourteen oligostilbenes were isolated from this extract on a fully automated semi-preparative HPLC system. Out of these, two pairs of dimers, one pair of trimers, two pairs of tetramers and a group of four tetramers with similar skeleton were identified as diastereoisomers. Their structures and configurations were established by spectroscopic methods. All isolated compounds were subjected to an LC-MS/MS to study their fragmentation patterns. The experiments were performed on a liquid chromatography-mass spectrometry (LC-MS) with electrospray-ionization (ESI) interface in positive mode. MS/MS spectra of each pure compound were recorded by direct infusion in identical conditions and their product ion spectra were analysed. Some subtle yet significant differences were observed between the spectra of oligostilbenes from the various diastereoisomeric series.

Effective Analysis of Dicyclanil in Lamb and Chicken Muscle using HPLCUV/Vis and LC/MS/MS

  • Kim, Byung-Ju;Myung, Seung-Woon
    • Mass Spectrometry Letters
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    • v.2 no.2
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    • pp.45-48
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    • 2011
  • The authors describe a method for monitoring dicyclanil levels in lamb and chicken muscle tissues. The devised procedure involves dicyclanyl extraction by SPE and its detection HPLC-UV/Vis and LC/MS/MS. The method was found to have LOD and LOQ values of $0.02\;mg\;kg^{-1}$ and $0.05\sim0.06\;mg\;kg^{-1}$, respectively. The intraday precision and an accuracy of spiked samples were found to have 2.3~10.4 RSD% and 80.9~105.7%, respectively.

Optimization of Solid Phase Extraction Method for Quantitative Analysis of Perfluorooctanoic Acid in Serum using Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Hyun-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.30-33
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    • 2014
  • A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

Simultaneous determination of seven major human cytochrome P450 activities using LC/MS/MS

  • Lee, Seung-Seok;Kim, Hae-Kyoung;Jin, Joon-Ki;Lee, Hye-Won;Kim, John;Lee, Hye-Suk
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.404.1-404.1
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    • 2002
  • A LC/MS/MS method for the simultaneous determination of the activities of seven major human drug-metabolizing cytochrome P450s (CYP3A4. CYP2D6. CYP2C9. CYP1A2, CYP2C19, CYP2A6. and CYP2C8) was developed. This method used an in vitro cocktail of specific substrates (midazolam. bufuralol. diclofenac, ethoxyresorufin. S-mephenYlOin. coumarin. and paclitaxel) and LC/MS/MS. The assay incubation time is 20 min and the analysis time is 8 min/sample. (omitted)

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LC-MS/MS-Based Comparative Investigation on Chemical Constituents of Six Aster Species Occurring in Korea

  • Kang, Kyo Bin;Lee, Dong Young;Sung, Sang Hyun
    • Natural Product Sciences
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    • v.27 no.4
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    • pp.257-263
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    • 2021
  • Aster species (Asteraceae) are widely distributed edible and medicinal plants, known to contain various specialized metabolites including polyphenols and saponins. However, systemic analysis on the chemical profiles of these plants have rarely been made. Here we analyzed the phytochemical constituents in leaves of 6 Aster species occurring in Korea, A. ageratoides, A. altaicus var. uchiyamae, A. glehnii, A. hispidus, A. incisus, and A. yomena, by applying a LC-MS/MS-based untargeted metabolomics approach. The analysis revealed that A. ageratoides, A. hispidus, and A. yomena are relatively rich in saponins most of which are expected to be previously unknown.