• Title/Summary/Keyword: quadrupole mass spectrometry

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Metabolic profiling and method validation of marker compounds from Saposhnikoviae Radix and Peucedani Japonici Radix (방풍, 식방풍의 대사체 프로파일링을 통한 지표성분 선정 및 분석법검증)

  • Choi, Bo-Ram;Yoon, Dahye;Kim, Geum-Soog;Han, Kyung-Sook;Choi, Doo Jin;Lee, Young-Seob;Hyun, Do Yoon;Lee, Dae Young
    • Journal of Applied Biological Chemistry
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    • v.63 no.4
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    • pp.393-399
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    • 2020
  • Saposhnikoviae Radix (SR) and Peucedani Japonici Radix (PR) have been used as the main traditional herbal medicines in Korea, China and Japan. In this study, ultra-performance liquid chromatography coupled to quadrupole time of flight mass spectrometry (UPLC-QTOF/MS)-based metabolomics was applied to evaluate the quality of SR and PR using the marker compounds. In the S-plot of SR and PR, 5-O-methylvisammioside and peucedanol were selected as a marker compound for SR and PR, respectively. Also, an UPLC method was established and well validated for marker compounds of SR and PR. These results suggested that the established analysis method could be used one of the good methods for the classification and quality assessment of SR and PR.

Study of Simultaneous Analysis of Indicator Components of DTP(Digital Textile Printing) Textile Products Using HPLC-MS/MS - Focusing on Natural Dyes - (HPLC-MS/MS를 활용한 DTP(Digital Textile Printing) 제품의 지표성분 동시분석법 연구 - 천연염료를 중심으로 -)

  • Lee, Wonkyoung;Sung, Eunji;Moon, Joung Ryul;Kim, Miji;Kim, Jonghoon
    • Fashion & Textile Research Journal
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    • v.23 no.6
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    • pp.844-851
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    • 2021
  • Due to the increase in consumers' interest about well-being, interest in eco-friendly products has been increasing due to the harmful effects of various harmful substances contained in textile products and environmental issues. As a result, natural dyes of less potential risk than synthetic dyes and digital textile printing(DTP) textile products with less environmental pollution are drawing attention. However, due to the lack of evaluation criteria for DTP textile products with natural ink and the nature of many colors are stacked layer by layer for dying, the need for simultaneous analysis is emerging. To evaluate whether the natural dye is derived from natural ingredients, the biocarbon content is analyzed. However, in the case of ink made using natural dyes and DTP textile products using natural ink, it is difficult to analyze the biocarbon content due to the limitation of the presence of a small amount of dye contained therein. In this study, we were shown the possibility of natural derived verification by cross-checking the analytes of natural dyes (Persicaria tinctoria, an indigo dye; Dactylopius coccus, a light red; and Curcum longa L., i.e., turmeric) and natural ink with HPLC-MS/MS. The coefficient of determination was 0.999 or higher, the limit of quantification was 0.647-3.664 ㎍/L and a %RSD of each indicator material was less than 10. Then, the extraction amount of natural dyes for five patterned fabrics was analyzed.

Evaluation of storage period of fresh ginseng for quality improvement of dried and red processed varieties

  • Zhang, Na;Huang, Xin;Guo, Yun-Long;Yue, Hao;Chen, Chang-Bao;Liu, Shu-Ying
    • Journal of Ginseng Research
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    • v.46 no.2
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    • pp.290-295
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    • 2022
  • Background: Dried and red ginseng are well-known types of processed ginseng and are widely used as healthy food. The dried and red ginseng quality may vary with the storage period of raw ginseng. Therefore, herein, the effect of the storage period of fresh ginseng on processed ginseng quality was evaluated through multicomponent quantification with statistical analysis. Methods: A method based on ultrahigh performance liquid chromatography coupled to triple quadrupole mass spectrometry in multiple-reaction monitoring mode (UPLC-MRM-MS) was developed for quantitation of ginsenosides and oligosaccharides in dried and red ginseng. Principal component analysis and partial least squares discriminant analysis were conducted to evaluate the dynamic distributions of ginsenosides and oligosaccharides after different storage periods. Results: Eighteen PPD, PPT and OLE ginsenosides and nine reducing and nonreducing oligosaccharides were identified and quantified. With storage period extension, the ginsenoside content in the processed ginseng increased slightly in the first 2 weeks and decreased gradually in the following 9 weeks. The content of reducing oligosaccharides decreased continuously as storage time extending, while that of the nonreducing oligosaccharides increased. Chemical conversions occurred during storage, based on which potential chemical markers for the storage period evaluation of fresh ginseng were screened. Conclusion: According to ginsenoside and oligosaccharide distributions, it was found that the optimal storage period was 2 weeks and that the storage period of fresh ginseng should not exceed 4 weeks at 0 ℃. This study provides deep insights into the quality control of processed ginseng and comprehensive factors for storage of raw ginseng.

DRY ETCHING CHARACTERISTICS OF INGAN USING INDUCTIVELY COUPLED $Cl_2/CHF_3,{\;}Cl_2/CH_4$ AND Cl_2/Ar PLASMAS.

  • Lee, D.H.;Kim, H.S.;G.Y. Yeom;Lee, J.W.;Kim, T.I.
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 1999.10a
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    • pp.59-59
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    • 1999
  • In this study, planer inductively coupled $Cl_2$ based plasmas were used to etch InGaN and the effects of plasma conditions on the InGaN etch properties have been characterized using quadrupole mass spectrometry(QMS) and optical emission spectroscopy(OES). As process conditions used to study the effects of plasma characteristics on the InGaN etch properties, $Cl_2$ was used as the main etch gas and $CHF_3,{\;}CH_4$, and Ar were used as additive gases. Operational pressure was varied from SmTorr to 3OmTorr, inductive power and bias voltage were varied from 400W to 800W and -50V to -250V, respectively while the substrate temperature was fixed at 50 centigrade. For the $Cl_2$ plasmas, selective etching of GaN to InGaN was obtained regardless of plasma conditions. The small addition of $CHF_3$ or Ar to $Cl_2$ and the decrease of pressure generally increased InGaN etch rates. The selective etching of InGaN to GaN could be obtained by the reduction of pressure to l5mTorr in $CI_2/IO%CHF_3{\;}or{\;}CI_2/IO%Ar$ plasma. The enhancement of InGaN etch rates was related to the ion bombardment for $CI_2/Ar$ plasmas and the formation of $CH_x$ radicals for $CI_2/CHF_3(CH_4)$ plasmas.

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Quantitative Analysis and Enantiomeric Separation of Ephedra Alkaloids in Ma Huang Related Products by HPLC-DAD and UPLC-MS/MS

  • Kyoung-Moon Han;Jinwoo Hwang;Sun Hee Lee;Boreum Park;Hyungil Kim;Sun Young Baek
    • Natural Product Sciences
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    • v.28 no.4
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    • pp.168-180
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    • 2022
  • Ephedra is a genus of the Ephedraceae family and is found in temperate regions, such as Central Asia and Europe. Among the various ephedra species, Ma Huang (Ephedra herb) is derived from the aerial parts of Ephedra sinica S tapf, Ephedra equisetina Bunge, and Ephedra intermedia Schrenk & C.A. Mey. Ma Huang contains various ephedra alkaloids, including (-)-ephedrine, (+)-pseudoephedrine, (-)-norephedrine, (+)-norpseudoephedrine, (-)-methylephedrine, and (+)-methylpseudoephedrine, which are found naturally as single enantiomers, although they can be prepared as racemates. Although the use of Ma Huang in foods is prohibited in Korea, products containing Ma Huang can be imported, and so it is necessary to develop a suitable analytical technique for the detection of Ma Huang in foods. Herein, we report the development of analytical methods for the detection of ephedra alkaloids in products containing Ma Huang. Following sample purification by solid phase extraction, quantitative analysis was performed using ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). Additionally, the enantiomers were successfully separated using HPLC-DAD. We successfully analyzed various food samples, where the ephedra alkaloids were qualitatively and quantitatively determined, and the enantiomers were separated. It is expected that these methods may contribute toward preventing the distribution of illegal products containing Ma Huang.

Discrimination of biological and artificial nicotine in e-liquid

  • Hyoung-Joon Park;Heesung Moon;Min Kyoung Lee;Min Soo Kim;Seok Heo;Chang-Yong Yoon;Sunyoung Baek
    • Analytical Science and Technology
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    • v.36 no.1
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    • pp.22-31
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    • 2023
  • As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R2 > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

Analysis of Anthocyanin Glycosides in Korean Mulberry Fruit Cultivars (한국산 오디 품종별 안토시아닌 배당체 성분 분석)

  • So Ah Kim;Ryeong Ha Kwon;Ju Hyung Kim;Hyemin Na;Ji Hae Lee;Soo-Muk Cho;Heon-Woong Kim
    • The Korean Journal of Food And Nutrition
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    • v.36 no.6
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    • pp.543-550
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    • 2023
  • Mulberry fruit is a superior source of polyphenols, especially anthocyanin, and has a long history of use as an edible fruit and traditional medicine. The anthocyanin composition of mulberry fruit from 15 Korean cultivars was analyzed by ultra-performance liquid chromatography diode array detector with quadrupole time of flight/mass spectrometry (UPLC-DAD-QToF/MS) based on a cyanin internal standard. The four glycosides were identified by comparison with authentic standards and published reports. The major anthocyanin was cyanidin 3-O-glucoside (71.7%), followed by cyanidin 3-O-rutinoside (26.6%). The minor components (total of 1.7%) were pelargonidin 3-O-glucoside and pelargonidin 3-O-rutinoside. The total anthocyanin content (mg/100 g, dry weight) of mulberry fruit varied by cultivar and ranged from 471.5±4.0 (Su Hong) to 4,700.2±54.0 (Gwa Sang2). Among the 15 cultivars examined, Gwa Sang2 showed the highest level of cyanidin 3-O-glucoside (3,133.4±32.6), which was 9-fold higher than that of Su Hong (351.5±3.4). In conclusion, anthocyanin profiles, including pelargonidin 3-O-glucoside and pelargonidin 3-O-rutinoside, were reported for the first time from 15 Korean mulberry fruit cultivars. The results will contribute valuable information on pharmaceutical properties, breeding superior mulberry cultivars, and food industries.

Metabolomic Profiles in Patients with Cervical Cancer Undergoing Cisplatin and Radiation Therapy

  • Seo-Yeon Choi;Suin Kim;Ji-Young Jeon;Min-Gul Kim;Sun-Young Lee;Kwang-Hee Shin
    • Biomolecules & Therapeutics
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    • v.32 no.3
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    • pp.379-389
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    • 2024
  • This study was aimed to evaluate endogenous metabolic changes before and after cisplatin and radiation therapy in patients with cervical cancer via untargeted metabolomic analysis using plasma samples. A total of 13 cervical cancer patients were enrolled in this study. Plasma samples were collected from each patient on two occasions: approximately one week before therapy (P1) and after completion of cisplatin and radiation therapy (P2). Of the 13 patients, 12 patients received both cisplatin and radiation therapy, whereas one patient received radiation therapy alone. The samples were analyzed using the Ultimate 3000 coupled with Q ExactiveTM Focus Hybrid Quadrupole-OrbitrapTM mass spectrometry (Thermo Fisher Scientific, Waltham, MA, USA). Chromatographic separation utilized a Kinetex C18 column 2.1×100 mm (2.6 ㎛) (Phenomenex, Torrance, CA, USA), and the temperature was maintained at 40℃. Following P2, there were statistically significant increases in the concentrations of indoxyl sulfate, phenylacetylglutamine, Lysophosphatidyethanolamine (LysoPE) (18:1), and indole-3-acetic acid compared with the concentrations observed at P1. Specifically, in the human papillomavirus (HPV) noninfection group, indoxyl sulfate, LysoPE (18:1), and phenylacetylglutamine showed statistically significant increases at P2 compared with P1. No significant changes in metabolite concentrations were observed in the HPV infection group. Indoxyl sulfate, LysoPE (18:1), phenylacetylglutamine, and indole-3-acetic acid were significantly increased following cisplatin and radiation therapy.

Biochemical Assessment of Deer Velvet Antler Extract and its Cytotoxic Effect including Acute Oral Toxicity using an ICR Mice Model (ICR 마우스 모델을 이용한 녹용 추출물의 생화학적 평가 및 급성 경구 독성을 포함한 세포 독성 효과)

  • Ramakrishna Chilakala;Hyeon Jeong Moon;Hwan Lee;Dong-Sung Lee;Sun Hee Cheong
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.430-441
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    • 2023
  • Velvet antler is widely used as a traditional medicine, and numerous studies have demonstrated its tremendous nutritional and medicinal values including immunity-enhancing effects. This study aimed to investigate different deer velvet extracts (Sample 1: raw extract, Sample 2: dried extract, and Sample 3: freeze-dried extract) for proximate composition, uronic acid, sulfated glycosaminoglycan, sialic acid, collagen levels, and chemical components using ultra-performance liquid chromatography-quadrupole-time-of-light mass spectrometry. In addition, we evaluated the cytotoxic effect of the deer velvet extracts on BV2 microglia, HT22 hippocampal cells, HaCaT keratinocytes, and RAW264.7 macrophages using the cell viability MTT assay. Furthermore, we evaluated acute toxicity of the deer velvet extracts at different doses (0, 500, 1000, and 2000 mg/kg) administered orally to both male and female ICR mice for 14 d (five mice per group). After treatment, we evaluated general toxicity, survival rate, body weight changes, mortality, clinical signs, and necropsy findings in the experimental mice based on OECD guidelines. The results suggested that in vitro treatment with the evaluated extracts had no cytotoxic effect in HaCaT keratinocytes cells, whereas Sample-2 had a cytotoxic effect at 500 and 1000 ㎍/mL on HT22 hippocampal cells and RAW264.7 macrophages. Sample 3 was also cytotoxic at concentrations of 500 and 1000 ㎍/mL to RAW264.7 and BV2 microglial cells. However, the mice treated in vivo with the velvet extracts at doses of 500-2000 mg/kg BW showed no clinical signs, mortality, or necropsy findings, indicating that the LD50 is higher than this dosage. These findings indicate that there were no toxicological abnormalities connected with the deer velvet extract treatment in mice. However, further human and animal studies are needed before sufficient safety information is available to justify its use in humans.

Electrospray ionization tandem mass fragmentation pattern of camostat and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (Camostat 및 분해산물 4-(4-guanidinobenzoyloxy)phenylacetic acid의 전자분무 이온화 텐덤 질량 fragmentation 패턴)

  • Kwon, Soon-Ho;Shin, Hye-Jin;Park, Ji-Myeong;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.78-84
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    • 2011
  • The fragmentation patterns of a serine protease inhibitor, camostat, and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (GBPA), were for the first time investigated by a triple quadrupole tandem mass spectrometry equipped with an electrospray source (ESI-MS/MS) in positive and/or negative ion mode under collision-induced dissociation (CID). The positive CID spectrum of camostat showed distinctly that the single bond (C-O) cleavage between carbonyl group and oxygen atom of the ester bonds of the compound favorably occurred and then the loss of N,N-dimethylcarbamoylmethyl group was more susceptible than that of guanidine moiety. In the positive ion CID spectrum of GBPA, the initial cleavage between the carbonyl group and oxygen atom of 4-guanidinobenzoyloxy group also occurred, yielding the most abundant fragment ion at m/z 145. On the other hand, the negative CID spectrum of GBPA characteristically showed the occurrence of the most abundant peak at m/z 226 resulting from the sequential neutral losses of $CO_2$ and HN=C=NH from the parent ion at m/z 312.