• 대한화장품학회지
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• 제35권1호
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• pp.11-17
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• 2009

스테로이드 함유 표시가 없는 화장품에서 항염증 효과가 있는 글루코코티코스테로이드인 베타메타손프로피오네이트 성분이 검출되었다. 이 화장품은 외용스프레이 및 샴푸로서 주성분으로 아연피리치온을 함유하는 것으로 표기되어 있었다. 화장품에서 스테로이드 구조와 활성을 갖는 물질의 존재를 확인하기 위하여 실리카겔 박층판을 이용한 박층크로마토그래프를 사용하였으며 이 성분을 분리하기 위해 high-performance liquid chromatography (HPLC)를 이용하여 확인 및 정량을 수행하였다. 분취용 HPLC를 이용하여 스테로이드를 함유한 것으로 판단되는 분획을 모은 다음 nuclear magnetic resonance (NMR) 및 mass spectrometry (MS)를 이용하여 스테로이드 성분을 확인하였다. 스테로이드 표준물질로 베타메타손 17-프로피오네이트 및 베타메타손 21-프로피오네이트를 합성하여 사용하였고 이 표준물질과 HPLC 크로마토그램을 비교하여 스테로이드 성분의 함량을 분석하였다. 이 방법으로 아연피리치온 제제와 같은 일부 시판 화장품에서 스테로이드 성분을 확인하였고 reversed-phase high-performance liquid chromatography (RP HPLC) 상의 유지시간 비교를 통하여 스테로이드 성분을 정량한 결과 시험한 총 8종의 화장품 시료 중 2개 제품에서 0.005 ${\sim}$ 0.02%의 베타메타손프로피오네이트가 검출되었다.

• Food Science and Biotechnology
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• 제18권5호
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• pp.1237-1242
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• 2009

Polymethoxylated flavones (PMFs) extracted from Citrus sinensis 'Jincheng' peel were characterized by chromatographic and spectroscopic techniques. Seven individual PMF were identified. 3, 3', 4', 5, 6, 7-hexamethoxyflavone (HEX), nobiletin (NOB), heptamethoxyflavone (HEP), 5-demethylnobiletin (DN), and tangeretin (TAN) were characterized through electrospray ionization mass spectrometry (ESI-MS) in positive mode of protonated molecular ions $[M+H]^+$, the diagnostic fragment ions, together with the UV-Vis spectra and high performance liquid chromatography (HPLC) elution order from literature data. Sinensetin (SIN) and tetramethyl-O-scutellarein (SCU) were isolated and identified through their MS, $^1H$ nuclear magnetic resonance (NMR) and UV-Vis spectral studies. The levels of PMFs in peels from different cultivars of citrus fruits grown in China were determined for the first time. The results showed that C. aurantium 'Bitter orange' peel was the most promising variety for HEP. C. sinensis peel was a good source for SIN and SCU.

• Journal of Biomedical and Translational Research
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• 제19권4호
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• pp.130-139
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• 2018

This study aimed to analyze a high-performance liquid chromatography (HPLC) separation using a pentafluorophenyl column of parent drug hydroxychloroquine (HCQ) and its active metabolite, desethylhydroxchloroquine (DHCQ) applying to determine bioequivalence of two different formulations administered to patients. A rapid, simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for bioanalysis of HCQ and its metabolite DHCQ in human whole blood using deuterium derivative $hydroxychloroquine-D_4$ as an internal standard (IS). A triple-quadrupole mass spectrometer was operated using electrospray ionization in multiple reaction monitoring (MRM) mode. Sample preparation involves a two-step precipitation of protein techniques. The removed protein blood samples were chromatographed on a pentafluorophenyl (PFP) column ($50mm{\times}4.6mm$, $2.6{\mu}m$) with a mobile phase (ammonium formate solution containing dilute formic acid) in an isocratic mode at a flow rate of 0.45 mL/min. The standard curves were found to be linear in the range of 2 - 500 ng/mL for HCQ; 2 - 2,000 ng/mL for DHCQ in spite of lacking a highly sensitive MS spectrometry system. Results of intra- and inter-day precision and accuracy were within acceptable limits. A run time of 2.2 min for HCQ and 2.03 min for DHCQ in blood sample facilitated the analysis of more than 300 human whole blood samples per day. Taken together, we concluded that the assay developed herein represents a highly qualified technology for the quantification of HCQ in human whole blood for a parallel design bioequivalence study in a healthy male.

• Journal of Microbiology and Biotechnology
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• 제25권11호
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• pp.1954-1959
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• 2015

Bacillus subtilis HM1 was isolated from the rhizosphere region of halophytes for its antifungal activity against Colletotrichum acutatum, the causative agent of anthracnose. Treatment of postharvest apples with the cell culture or with a cell-free culture supernatant reduced disease severity 80.7% and 69.4%, respectively. Both treatments also exhibited antifungal activity against various phytopathogenic fungi in vitro. The antifungal substances were purified and analyzed by acid precipitation, gel filtration, high-performance liquid chromatography, and matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS). Three compounds were identified as fengycin, iturin, and surfactin. The MALDI-TOF/TOF mass spectrum revealed the presence of cyclized fengycin homologs A and B, which were distinguishable on the basis of the presence of either alanine or valine, respectively, at position 6 of the peptide sequence. In addition, the cyclized structure of fengycin was shown to play a critical role in antifungal activity.

• 분석과학
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• 제17권3호
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• pp.263-270
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• 2004

알킬페놀에톡실레이트 (APEO)는 주로 비이온성 계면활성제로 쓰이고 있으며 세제, 액체연료 및 농약에도 이용이 되고 있다. APEO 자체는 독성물질로 분류되어 있지 않지만, 그 대사생성물질인 단사슬 APEO, 알킬페놀 및 카르복실 유도체등은 폐수 또는 음용수를 염소처리하는 동안 mutagenic ring halogenated derivative를 생성한다. 이들 생성물들은 estrogenic effect를 나타내기 때문에 APEO를 제한 또는 규제하고 있는 추세이다. 본 연구에서는 APEO의 대사체로서 단사슬 APEO 인 4-nonylphenol-di-ethoxylate (NP2EO), 4-octylphenol-di-ethoxylate (OP2EO)를 분석하기 위해서 p-n-nonylphenol-di-ethoxylate-ring-$^{13}C_6$을 내부표준물질로 사용하여 HPLC/ESI/MS를 이용하여 분석하였다. 분석조건은 이온화 용매인 trifluoroacetic acid가 $10{\mu}M$이 되도록 각각 물과 메탄올에 첨가시켜 사용하였다. 물시료 1 L에 진한 황산을 이용하여 pH를 2이하로 조정한 후, 아세톤, 메탄올 및 물 (pH 2)로 활성화시킨 Sep-Pak $C_{18}$에 loading 시킨 후 아세톤으로 용출하여 시료용액으로 하였다. 이 방법으로 농도범위가 20 ~ 500 ng/L 내에서 검량선의 직선성은 r=0.999 (OP2EO)와 0.990 (NP2EO)였으며, 검출한계는 OP2EO는 20 ng/L, NP2EO는 50 ng/L 이었다. 정확도 및 정밀도는 85.8~122.1% 및 8.2~18.8 %로 좋은 결과를 나타냈다. 이 방법은 환경시료로부터 미량의 APEO를 분석하는데 사용될 수 있고, APEO 오염실태 조사에 응용될 수 있을 것으로 사료된다.

• 생약학회지
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• 제38권2호통권149호
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• pp.123-127
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• 2007

Aristolochic acid (AA) included in the plants Aristolochiaceae have been well known to be nephrotoxic and carcinogenic inducer and to cause renal disease such as Chinese Herb Nephropathy (CHN). In this study, we used a high performance liquid chromatopaphy-mass spectrometry (HPLC-MS) under the positive ion detection mode for the quantitative change of aristolochic acid-I and-II (AA-I and AA-II) in Aristolochiaceae (Aristolochia contorta Bunge, Aristolochia debilis Sieb. et Zucc., Aristolochia fangchi Wu), some related plants (Cocculus trilobus De candolle, Inula helenium Linne, Saussurea lappa Clarke), and its prescriptions (防己茯笭湯, 定喘散) with or without processing. Here, the processing methods and prescriptions in oriental medicine were generally used to alleviate toxicity or alter property of herbal medicines. However, the concentrations of AA-I and AA-II were highly determined in processed material extracts rather than unprocessed those, not measured in some related plants. Also, the concentrations of AA-I and AA-II even at the prescriptions mixed the plants of Aristolochiaceae were detected to range from 0.73 to 2.53 ppm. Thus, the present results suggest that the content of AA-I and AA-II contained to plants of Aristolochiaceae was not reduced by the processing methods or prescriptions which can induce the physico-chemical change and pharmacological transformation in traditional herbal medicines.

• Bulletin of the Korean Chemical Society
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• 제34권6호
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• pp.1684-1688
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• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

• Journal of Ginseng Research
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• 제42권2호
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• pp.149-157
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• 2018

Background: Panax notoginseng leaves (PNL) exhibit extensive activities, but few analytical methods have been established to exclusively determine the dammarane triterpene saponins in PNL. Methods: Ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC/Q-TOF MS) and HPLC-UV methods were developed for the qualitative and quantitative analysis of ginsenosides in PNL, respectively. Results: Extraction conditions, including solvents and extraction methods, were optimized, which showed that ginsenosides Rc and Rb3, the main components of PNL, are transformed to notoginsenosides Fe and Fd, respectively, in the presence of water, by removing a glucose residue from position C-3 via possible enzymatic hydrolysis. A total of 57 saponins were identified in the methanolic extract of PNL by UPLC/Q-TOF MS. Among them, 19 components were unambiguously characterized by their reference substances. Additionally, seven saponins of PNL-ginsenosides Rb1, Rc, Rb2, and Rb3, and notoginsenosides Fc, Fe, and Fd-were quantified using the HPLC-UV method after extraction with methanol. The separation of analytes, particularly the separation of notoginsenoside Fc and ginsenoside Rc, was achieved on a Zorbax ODS C8 column at a temperature of $35^{\circ}C$. This developed HPLC-UV method provides an adequate linearity ($r^2$ > 0.999), repeatability (relative standard deviation, RSD < 2.98%), and inter- and intraday variations (RSD < 4.40%) with recovery (98.7-106.1%) of seven saponins concerned. This validated method was also conducted to determine seven components in 10 batches of PNL. Conclusion: These findings are beneficial to the quality control of PNL and its relevant products.

• Journal of Applied Biological Chemistry
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• 제64권2호
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• pp.141-151
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• 2021

Insects affect crop harvest yield and quality, making plant response mechanisms to insect herbivores a heavily studied topic. However, analysis of plant responses to honeybees is rare. In this study, comprehensive metabolic profiling of Arabidopsis thaliana exposed to honeybees was performed to investigate which metabolites were changed by the insect. A total of 85 metabolites-including chlorophylls, carotenoids, glucosinolates, policosanols, tocopherols, phytosterols, β-amyrin, amino acids, organic acids, sugars, and starch-were identified using high performance liquid chromatography, gas chromatography-mass spectrometry, and gas chromatography-time-of-flight mass spectrometry. The metabolite profiling analysis of Arabidopsis exposed to honeybees showed higher levels of stress-related metabolites. The levels of glucosinolates (glucoraphanin, 4-methoxyglucobrassicin), policosanols (eicosanol, docosanol, tricosanol, tetracosanol), tocopherols (β-tocopherol, γ-tocopherol), putrescine, lysine, and sugars (arabinose, fructose, glucose, mannitol, mannose, raffinose) in Arabidopsis exposed to honeybees were higher than those in unexposed Arabidopsis. Glucosinolates act as defensive compounds against herbivores; policosanols are components of plant waxes; tocopherols act as an antioxidant; and putrescine, lysine, and sugars contribute to stress regulation. Our results suggest that Arabidopsis perceives honeybees as a stress and changes its metabolites to overcome the stress. This is the first step to determining how Arabidopsis reacts to exposure to honeybees.

• Environmental Analysis Health and Toxicology
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• 제29권
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• pp.18.1-18.9
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• 2014

Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.