• Journal of the Society of Cosmetic Scientists of Korea
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• v.35 no.1
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• pp.11-17
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• 2009

Betamethasone propionate, an anti-inflammatory glucocorticosteroid, was detected in cosmetics with no indication on the label of this compound as an ingredient. The product was formulated as a topical spray or shampoo and labeled to contain zinc pyrithione as the active ingredient. A thin-layer chromatographic analysis was carried out on silica gel plates to provide a first indication about the presence of a compound with steroid structure and reactivity; then high-performance liquid chromatography (HPLC) separation allowed the identification of the corticosteroid agent and its quantification. To identify the corticosteroid agent from these commercial samples we collected the fractions suspected to have ketol steroids by prep HPLC and identified the compound as betamethasone propionate by NMR and MS spectrometry. Then we synthesized the standard for the betamethasone 17-propionate and 21-propionate and quantitate the corticosteroids from the sample by HPLC with that standards. By this method we identified the corticosteroid compounds from some commercial cosmetics such as zinc pyrithione sprays. The finding of betamethasone propionate in the products was shown by comparison to an authenticated standard of betamethasone propionate by retention time on reverse-phase HPLC. Two of the tested products contained betamethasone propionate at the levels of 0.005 ${\sim}$ 0.02% and the others were free of betamethasone propionate.

• Food Science and Biotechnology
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• v.18 no.5
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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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• v.19 no.4
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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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• v.25 no.11
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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.

• Analytical Science and Technology
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• v.17 no.3
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• pp.263-270
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• 2004

A method is described for the analysis of short-chain alkylphenol ethoxylates (APEOs), 4-octylphenol-di-ethoxylate (OP2EO) and 4-nonylphenol-di-ethoxylate (NP2EO), in drinking water or wastewater using reversed phase high-performance liquid chromatography with electrospray ionization mass spectrometry. The solvent system was water and methanol containing $10{\mu}M$ trifluoroacetic acid as an ionization solvent. We acidified 1 L of water samples to less than pH 2 with concentrated $H_2SO_4$ and loaded onto Sep-Pak $C_{18}$, and eluted with acetone. The calibration of OP2EO and NP2EO was performed for the concentration range from 20 to 500 ng/L and the correlation coefficients were 0.999 and 0.990, respectively. The limits of detection were 20 ng/L (OP2EO) and 50 ng/L (NP2EO) at a signal-to-noise ratio of 3. Accuracy and precision of this analytical method were 85.8 ~ 122.1% and 8.2 ~ 18.8%, respectively. The proposed method allowed a sensitive and rapid detection of OP2EO and NP2EO and it could be applied for monitoring of APEOs from environmental samples.

• Korean Journal of Pharmacognosy
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• v.38 no.2 s.149
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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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• v.34 no.6
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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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• v.42 no.2
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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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• v.64 no.2
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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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• v.29
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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.