• 제목/요약/키워드: Liquid Chromatography-tandem Mass Spectrometry

검색결과 400건 처리시간 0.027초

유통 한약재 초과(草果) 중 벤조피렌 오염실태 조사 (A Survey on Benzo(a)pyrene Contamination in Amomum Tsao-ko Fruit of Medicinal Herbs)

  • 황경화;염미숙;이희정;조아름;최은정;허명제;권문주
    • 생약학회지
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    • 제51권2호
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    • pp.146-150
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    • 2020
  • Amomum Tsao-ko used as a traditional oriental herbal medicine, is indigenous to several Asia countries. This study was carried out to investigate the contamination by Benzo(a)pyrene in Amomum Tsao-ko Fruit of Medicinal Herbs. 20 samples of Amomum Tsao-ko Fruit were evaluated for the Benzo(a)pyrene contamination. They were analyzed for Benzo(a)pyrene using high-performance liquid chromatogrphy(HPLC)-fluorescence detection and the positive samples were confirmed using gas chromatography tandem mass spectrometry. The levels of Benzo(a)pyrene were from 9.2 to 95.5 ㎍/kg and the average was 40.6 ㎍/kg. There are no Benzo(a)pyrene standards for Amomum Tsao-ko Fruit of Medicinal Herbs. These data will be used as a basic data for the future legislation on the regulation and control of benzo(a)pyrene of Amomum Tsao-ko Fruit of Medicinal Herbs.

LC/MS/MS를 이용한 석류추출물 중의 에스트로겐 분석 (Analysis of Estrogen in Pomegranate Extract by Solid Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry)

  • 금은주;권도형;신혜승
    • 한국식품위생안전성학회지
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    • 제25권1호
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    • pp.79-82
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    • 2010
  • 석류는 오래전부터 임상치료 및 식품원료로 사용되었으며 많은 피토에스트로겐 성분을 함유하고 있다. 그 성분으로는 에스트론, 에스트라디올, 에스트리올, 베타-시토스테롤, 엘라그산 등이 였으며 이러한 성분으로 인해 과즙, 껍질, 오일 등은 약한 에스트로겐 활성을 나타낸다고 보고되었으며, 이로 인해 석류는 여성 갱년기 치료용 원료로 많이 사용되고 있다. 그러나 에스트로겐 성분의 존재 유무에 대한 견해의 차이가 나타나고 있어 본 연구는 LC/MS/MS를 이용하여 석류추출물 중의 에스트로겐 분석을 통해 이를 확인하고자 하였으며, 간편하고 정확한 분석법을 모색하고자 하였다. 3개 롯트 시료의 에스트로겐을 분석한 결과, 에스트론 83.5ppb, 에스트라디올 10.9ppb 및 에스트리올 38.6ppb로 검출되었다.

Establishment of an analytical method for butaphosphan (BTP), a stress-attenuating agent, and its application in the preliminary pharmacokinetic evaluation of residues in olive flounder Paralichthys olivaceus

  • Lee, Ji-Hoon;Bae, Jun Sung;Lee, Chae Won;Yang, Chan Yeong;Choi, Ji-Sung;Choi, Sang-Hoon;Kang, Yue-Jai;Park, Kwan Ha
    • Fisheries and Aquatic Sciences
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    • 제23권4호
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    • pp.10.1-10.10
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    • 2020
  • Background: Butaphosphan (BTP) has recently been introduced into the Korean aquaculture sector as a stressattenuating agent. In this study, a sensitive chemical analytical method was established for the detection of BTP in the olive flounder (Paralichthys olivaceus) tissues. Methods: Utilizing a method employing liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS), detection sensitivity, specificity, and precision were satisfactorily established. Temporal changes in the BTP plasma and muscle concentrations were assessed after a single intramuscular injection of BTP (50 and 150 mg/kg) to the olive flounder maintained at 13 ℃ or 22 ℃. Results: High BTP plasma levels were achieved immediately after the injection, and the drug was rapidly eliminated. Additionally, plasma BTP levels were markedly dependent on the elimination rate, which, in turn, seemed dependent on the water temperature, with the drug elimination half-life and mean residence time significantly shorter at 22 ℃ than 13 ℃. Overall, muscle BTP levels were markedly lower than the plasma levels. Notably, muscle levels were not influenced by water temperatures. Muscle BTP concentrations were used to estimate the necessary withdrawal period for drugs used in food fish, with BTP levels maintained far below the possible hazardous limit. Conclusions: In conclusion, the established LC-MS/MS method can be used for BTP residue detection with high sensitivity and reproducibility.

무균조제 항암제 취급의 안전관리 (Assessment of Occupational Exposure to Antineoplastic Agents in a Healthcare Setting)

  • 이수미;정선영;임현정;박효정;이수연;전은용;손기호
    • 약학회지
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    • 제55권2호
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    • pp.81-90
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    • 2011
  • Most antineoplastic agents are nonselective in their mechanism of action, affecting noncancerous as well as cancerous cells, and resulting in acute effects such as irritation of mucous membranes and chronic effects such as genotoxicity, teratogenicity, and carcinogenicity. Healthcare workers occupationally exposed to antineoplastic agents are at risk. The present study aimed to develop and apply methods to monitor occupational exposure to antineoplastic agents, using cyclophosphamide (CP) as the model compound. To monitor environmental and biological exposure, potentially contaminated surfaces were wiped and 24 hour urine samples were collected from workers. Liquid chromatography combined with tandem mass spectrometry was performed, with a limit of detection of 0.05 ng/ml. Measurable amounts of CP were detected on 92% of the sampled surfaces, with a geometric mean of 175.22 $ng/m^2$. Despite the environmental contamination of the model compound, CP was below the detection limit in all urine samples. If workplace contamination cannot be completely avoided, it is importance to reduce exposure to the lowest possible levels. To this aim, efforts to minimize occupational exposure along with biological and environmental monitoring are required. The standardized sampling techniques, and specific and sensitive analytical methods reported in this study may be helpful in assessing occupational exposure and devising strategies to reduce exposure.

Ginsenosides analysis of New Zealand-grown forest Panax ginseng by LC-QTOF-MS/MS

  • Chen, Wei;Balan, Prabhu;Popovich, David G.
    • Journal of Ginseng Research
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    • 제44권4호
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    • pp.552-562
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    • 2020
  • Background: Ginsenosides are the unique and bioactive components in ginseng. Ginsenosides are affected by the growing environment and conditions. In New Zealand (NZ), Panax ginseng Meyer (P. ginseng) is grown as a secondary crop under a pine tree canopy with an open-field forest environment. There is no thorough analysis reported about NZ-grown ginseng. Methods: Ginsenosides from NZ-grown P. ginseng in different parts (main root, fine root, rhizome, stem, and leaf) with different ages (6, 12, 13, and 14 years) were extracted by ultrasonic extraction and characterized by Liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry. Twenty-one ginsenosides in these samples were accurately quantified and relatively quantified with 13 ginsenoside standards. Results: All compounds were separated in 40 min, and a total of 102 ginsenosides were identified by matching MS spectra data with 23 standard references or published known ginsenosides from P. ginseng. The quantitative results showed that the total content of ginsenosides in various parts of P. ginseng varied, which was not obviously dependent on age. In the underground parts, the 13-year-old ginseng root contained more abundant ginsenosides among tested ginseng samples, whereas in the aboveground parts, the greatest amount of ginsenosides was from the 14-year-old sample. In addition, the amount of ginsenosides is higher in the leaf and fine root and much lower in the stem than in the other parts of P. ginseng. Conclusion: This study provides the first-ever comprehensive report on NZ-grown wild simulated P. ginseng.

A prebiotic fiber increases the formation and subsequent absorption of compound K following oral administration of ginseng in rats

  • Kim, Kyung-Ah;Yoo, Hye Hyun;Gu, Wan;Yu, Dae-Hyung;Jin, Ming Ji;Choi, Hae-Lim;Yuan, Kathy;Guerin-Deremaux, Laetitia;Kim, Dong-Hyun
    • Journal of Ginseng Research
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    • 제39권2호
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    • pp.183-187
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    • 2015
  • Background: Gut microflora play a crucial role in the biotransformation of ginsenosides to compound K (CK), which may affect the pharmacological effects of ginseng. Prebiotics, such as NUTRIOSE, could enhance the formation and consequent absorption of CK through the modulation of gut microbial metabolic activities. In this study, the effect of a prebiotic fiber (NUTRIOSE) on the pharmacokinetics of ginsenoside CK, a bioactive metabolite of ginsenosides, and its mechanism of action were investigated. Methods: Male Sprague-Dawley rats were given control or NUTRIOSE-containing diets (control diet + NUTRIOSE) for 2 wk, and ginseng extract or vehicle was then orally administered. Blood samples were collected to investigate the pharmacokinetics of CK using liquid chromatography-tandem mass spectrometry. Fecal activities that metabolize ginsenoside Rb1 to CK were assayed with fecal specimens or bacteria cultures. Results: When ginseng extract was orally administered to rats fed with 2.5%, 5%, or 10% NUTRIOSE containing diets, the maximum plasma concentration ($C_{max}$) and area under the plasma concentration-time curve values of CK significantly increased in a NUTRIOSE content-dependent manner. NUTRIOSE intake increased glycosidase activity and CK formation in rat intestinal contents. The CK-forming activities of intestinal microbiota cultured in vitro were significantly induced by NUTRIOSE. Conclusion: These results show that prebiotic diets, such as NUTRIOSE, may promote the metabolic conversion of ginsenosides to CK and the subsequent absorption of CK in the gastrointestinal tract and may potentiate the pharmacological effects of ginseng.

Effect of a soluble prebiotic fiber, NUTRIOSE, on the absorption of ginsenoside Rd in rats orally administered ginseng

  • Kim, Kyung-Ah;Yoo, Hye Hyun;Gu, Wan;Yu, Dae-Hyung;Jin, Ming Ji;Choi, Hae-Lim;Yuan, Kathy;Guerin-Deremaux, Laetitia;Kim, Dong-Hyun
    • Journal of Ginseng Research
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    • 제38권3호
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    • pp.203-207
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    • 2014
  • Background: There is limited understanding of the effect of dietary components on the absorption of ginsenosides and their metabolites into the blood. Methods: This study investigated the pharmacokinetics of the ginseng extract and its main constituent ginsenoside Rb1 in rats with or without pretreatment with a prebiotic fiber, NUTRIOSE, by liquid chromatography tandem mass spectrometry. When ginsenoside Rb1 was incubated with rat feces, its main metabolite was ginsenoside Rd. Results: When the intestinal microbiota of rat feces were cultured in vitro, their ginsenoside Rd-forming activities were significantly induced by NUTRIOSE. When ginsenoside Rb1 was orally administered to rats, the maximum plasma concentration (Cmax) and area under the plasma drug concentratione-time curve (AUC) for the main metabolite, ginsenoside Rd, were $72.4{\pm}31.6ng/mL$ and $663.9{\pm}285.3{\mu}g{\cdot}h/mL$, respectively. When the ginseng extract (2,000 mg/kg) was orally administered, Cmax and AUC for ginsenoside Rd were $906.5{\pm}330.2ng/mL$ and $11,377.3{\pm}4,470.2{\mu}g{\cdot}h/mL$, respectively. When ginseng extract was orally administered to rats fed NUTRIOSE containing diets (2.5%, 5%, or 10%), Cmax and AUC were increased in the NUTRIOSE receiving groups in a dose-dependent manner. Conclusion: These findings reveal that intestinal microflora promote metabolic conversion of ginsenoside Rb1 and ginseng extract to ginsenoside Rd and promote its absorption into the blood in rats. Its conversion may be induced by prebiotic diets such as NUTRIOSE.

Identification of Glutathione Conjugates of 2, 3-Dibromopropene in Male ICR Mice

  • Lee Sang Kyu;Baik Seo Yeon;Jeon Tae Won;Jun In Hye;Kim Ghee Hwan;Jin Chun Hua;Lee Dong Ju;Kim Jun Kyou;Yum Young Na;Jeong Tae Cheon
    • Archives of Pharmacal Research
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    • 제29권2호
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    • pp.172-177
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    • 2006
  • Hepatotoxic potential of 2, 3-dibromopropene (2, 3-DBPE) and its conjugation with glutathione (GSH) were investigated in male ICR mice. Treatment of mice with 20, 50, and 100 mg/kg of 2, 3-DBPE for 24 h caused elevation of serum alanine aminotransferase and aspartate aminotransferase activities. The hepatic content of GSH was not changed by 2, 3-DBPE. Meanwhile, the GSH content was slightly reduced when mice were treated with 2, 3-DBPE for 6 h and significantly increased 12 h after the treatment. Subsequently, a possible formation of GSH conjugate of 2, 3-DBPE was investigated in vivo. After the animals were treated orally with 20, 50, and 100 mg/kg of 2, 3-DBPE, the animals were subjected to necropsy 6, 12, and 24 h later. A conjugate of S-2-bromopropenyl GSH was identified in liver and serum treated with 100 mg/kg of 2, 3-DBPE by using liquid chromatography-electrospray ionization tandem mass spectrometry. The protonated molecular ions $[M+H]^+$ of S-2-bromopropenyl GSH were observed at m/z 425.9 and 428.1 in the positive ESI spectrum with a retention time of 6.35 and 6.39 min, respectively. In a time-course study in livers following an oral treatment of mice with 100 mg/kg of 2, 3-DBPE for 6, 12, and 24 h, the 2, 3-DBPE GSH conjugate was detected maximally 6 h after the treatment. The present results suggested that 2, 3-DBPE-induced hepatotoxicity might be related with the production of its GSH conjugate.

Tacrolimus의 혈중농도측정법 비교 및 간이식환자에서의 집단 약동학 (Comparison of Analytical Methods of Tacrolimus in Plasma and Population Pharmacokinetics in Liver Transplant Recipients)

  • 김은영;강원구;곽혜선
    • 한국임상약학회지
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    • 제18권1호
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    • pp.60-67
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    • 2008
  • This study aimed to compare a microparticle enzyme immunoassay (MEIA) with a liquid chromatography-tandem mass spectrometry (LC/MS/MS) technique for the measurement of tacrolimus concentrations in adult liver transplant recipients, to investigate how the assay choice influenced the population pharmacokinetics of tacrolimus and to identify patient characteristics that affected pharmacokinetic parameters in each assay. Tacrolimus concentrations from 29 liver (n=52 paired-samples) transplant recipients measured by both MEIA and LC/MS/MS were used to evaluate the performance of these methods in the clinical setting. Tacrolimus pharmacokinetics was studied independently using MEIA and LC/MS/MS data in 70 adult patients using a population approach performed with NONMEM. Patient characteristics which influenced pharmacokinetic parameters in each assay were compared. The relation between LC/MS/MS and MEIA measurements was best described by the regression equation MEIA=1.465*LC/MS/MS-1.336 (r=0.91). Multiple linear regression analysis showed significant inverse relationships between assay difference and hematocrit (Hct) (p<0.025) in liver graft recipients. In MEIA, the population estimate of tacrolimus CL/F and apparent volume of distribution (Vd/F) were found to be 10.1 L/h and 226 L, and in LC/MS/MS, 13 L/h and 305 L respectively. Neither patient's age, weight, gender, grafted hepatic weight, albumin concentration, nor markers of liver function influenced tacrolimus CL/F The final model of CL/F was found to be 10.1+(Hct/Hct mean)$^{12.0}$ in MEIA and 13+(1+Hct/578) in LC/MS/MS indicating that CL/F was influenced by hematocrit.

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Remarkable impact of steam temperature on ginsenosides transformation from fresh ginseng to red ginseng

  • Xu, Xin-Fang;Gao, Yan;Xu, Shu-Ya;Liu, Huan;Xue, Xue;Zhang, Ying;Zhang, Hui;Liu, Meng-Nan;Xiong, Hui;Lin, Rui-Chao;Li, Xiang-Ri
    • Journal of Ginseng Research
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    • 제42권3호
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    • pp.277-287
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    • 2018
  • Background: Temperature is an essential condition in red ginseng processing. The pharmacological activities of red ginseng under different steam temperatures are significantly different. Methods: In this study, an ultrahigh-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry was developed to distinguish the red ginseng products that were steamed at high and low temperatures. Multivariate statistical analyses such as principal component analysis and supervised orthogonal partial least squared discrimination analysis were used to determine the influential components of the different samples. Results: The results showed that different steamed red ginseng samples can be identified, and the characteristic components were 20-gluco-ginsenoside Rf, ginsenoside Re, ginsenoside Rg1, and malonyl-ginsenoside Rb1 in red ginseng steamed at low temperature. Meanwhile, the characteristic components in red ginseng steamed at high temperature were 20R-ginsenoside Rs3 and ginsenoside Rs4. Polar ginsenosides were abundant in red ginseng steamed at low temperature, whereas higher levels of less polar ginsenosides were detected in red ginseng steamed at high temperature. Conclusion: This study makes the first time that differences between red ginseng steamed under different temperatures and their ginsenosides transformation have been observed systematically at the chemistry level. The results suggested that the identified chemical markers can be used to illustrate the transformation of ginsenosides in red ginseng processing.