• 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.

• Analytical Science and Technology
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• v.32 no.2
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• Journal of the Mineralogical Society of Korea
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• v.16 no.1
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• pp.1-17
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• 2003

The chemical composition of the arsenopyrite Ib adjoining“triple mutual contact”arsenopyrite + pyrite + hexagonal pyrrhotite may serve as a useful geothermometer in Stage II. In this study it corresponds to temperature T=33$0^{\circ}C$ and f( $S_2$)=10$^{-9.5}$ atm. And the pyrite-hexagonal pyrrhotite buffer curve indicates the probable range of the two variables; T= 315∼345$^{\circ}C$, and f( $S_2$)=10$^{-1}$0.5/∼10$^{-9}$ atm. The present antimony-bearing arsenopyrite (arsenopyrite Ic) is characterized by relatively high content of antimony, ranging from 4.95 to 8.91 percent Sb by weight and excess of iron and deficiency of anions are evident. Such a high antimonian arsenopyrite has never been known within single grain. But being the high content of antimony as in the arsenopyrite Ic, it does not serve as a geothermometer. The results of microprobe analyses for four pairs of asenopyrite and sphalerite in Stage III indicate the temperature range from 310 to 34$0^{\circ}C$, and sulphur fugacity range from 10$^{-10}$ ∼10$^{-9}$ atm. These values seem to correspond with those inferred from the Fe-As-S system.m..

• 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.

• Korean Journal of Clinical Pharmacy
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• v.16 no.1
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• pp.23-27
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• 2006

Doxorubicin (DXR) is a type of anti-cancer drug called an 'anthracycline glycoside', It works by impairing DNA synthesis, a crucial feature of cell division, and thus is able to target rapidly dividing cells. Doxorubicin is a very serious anti-cancer medication with definite potential to do great harm as well as great good. A liquid chromatography-tandem mass spectroscopy (LC-MS/MS) method was developed to identify and quantify DXR in small-volume biological samples. After the addition of internal standard (IS, $5{\mu}L\;of\;1{\mu}M/ml$ daunorubicin methanol solution) into the serum sample, the drug and IS were extracted by methanol. Following vortex for a 1min and centrifugation at 15,000g for 10 min the organic phase was transferred and evaporated under a vacuum. The residue was reconstituted with $350{\mu}L$ of mobile phase and $10{\mu}L$ was injected into C18 column with mobile phase composed of 0.05M ammonium acetate (0.1 M acetic acid adjusted to pH 3.5) and acetonitrile (40:60, v/v). The flow rate was kept constant at $350{\mu}L/min$. The ions were quantified in the multiple reaction mode (MRM), using positive ions, on a triple quadrupole mass spectrometer. The lower limits of quantification for Doxorubicin in plasma and small tissues were approximately 0.5 ng/mL and 0.5 ng/mL respectively. Intra- and inter-assay accuracy (% of nominal concentration) and precision (% CV) for all analytes were within 15%, respectively.

• Journal of the korean academy of Pediatric Dentistry
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• v.45 no.4
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• pp.455-463
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• 2018

The purpose of this study was to evaluate the effect of the intracanal medicaments on the push-out bond strength of the calcium silicate-based materials. Forty extracted single-root human mandibular premolars were sectioned below cementoenamel junction. Standardized root canal dimension was obtained with a parallel post drill. The specimens were randomly divided into a control group (no medicament), and experimental groups received medicaments with either CH (calcium hydroxide), DAP (double antibiotic paste; a mixture of ciprofloxacin and metronidazole), or TAP (triple antibiotic paste; a mixture of minocycline, ciprofloxacin and metronidazole). Following removal of medicaments with irrigation, roots were cut into sections with 1-mm-thickness. Thereafter, calcium silicate-based materials are applied to the specimens : (i) ProRoot MTA$^{(R)}$ and (ii) Biodentine$^{(R)}$. A push-out bond strength was measured and each specimen was examined to evaluate failure mode. Intracanal medication using CH significantly increased the bond strength to the root dentin. But there are no significant differences on the bond strength of ProRoot MTA$^{(R)}$ or Biodentine$^{(R)}$ among TAP, DAP and control groups. The dislodgement resistance of Biodentine$^{(R)}$ from root dentin was significantly higher than that of ProRoot MTA$^{(R)}$ regardless of the type of intracanal medicaments.

• Journal of Ginseng Research
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• v.44 no.1
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• pp.105-114
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• 2020

Background: Exploring the pharmacokinetic (PK) changes of various active components of single herbs and their combinations is necessary to elucidate the compatibility mechanism. However, the lack of chemical standards and low concentrations of multiple active ingredients in the biological matrix restrict PK studies. Methods: A putative multiple reaction monitoring strategy based on liquid chromatography coupled with mass spectrometry (LC-MS) was developed to extend the PK scopes of quantification without resorting to the use of chemical standards. First, the compounds studied, including components with available reference standard (ARS) and components lacking reference standard (LRS), were preclassified to several groups according to their chemical structures. Herb decoctions were then subjected to ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry analysis with appropriate collision energy (CE) in MS² mode. Finally, multiple reaction monitoring transitions transformed from MS² of ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry were used for ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometry to obtain the mass responses of LRS components. LRS components quantification was further performed by developing an assistive group-dependent semiquantitative method. Results: The developed method was exemplified by the comparative PK process of single herbs Radix Ginseng (RG), Radix Polygala (RP), and their combinations (RG-RP). Significant changes in PK parameters were observed before and after combination. Conclusion: Results indicated that Traditional Chinese Medicine combinations can produce synergistic effects and diminish possible toxic effects, thereby reflecting the advantages of compatibility. The proposed strategy can solve the quantitative problem of LRS and extend the scopes of PK studies.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.327-333
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• 2014

A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

• The Journal of the Petrological Society of Korea
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• v.19 no.3
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• pp.227-244
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• 2010

Abundant spinel lherzolite xenoliths showing distinctively different textural types such as protogranular, porphyroclastic, and mylonitic texture are trapped in the basaltic rocks from southeastern part of Jeju Island. These xenoliths show the textural spectrum from coarse-grained protogranular through porphyroclastic with bimodal grain size to fine-grained and foliated mylonitic texture. They tend to decrease in grain sizes and show more linear grain boundaries and more frequent triple junctions from protogranular through porphyroclastic to mylonitic. Spinel has different occurrence mode according the textural type. Spinel is always associated with orthopyroxene in protogranular texture, whereas it is scattered and independent of orthopyroxene in mylonitic texture. Additionally, porphyroblast from porphyroclastic and mylonitic textures has internal deformation features such as kink band, undulatory extinction and curved lamella, whereas neoblast is strain-free. These textural features indicate increasing degree of static/dynamic recrystallization from protogranular through porphyroclastic to mylonitic texture. The mg#[$=100{\times}Mg/(Mg+Fe_t)$] of olivine, orthopyroxene and clinopyroxene is relatively constant (ol: 88-91; opx: 89-92; cpx: 89-92) regardless of textural differences. The mg# of constituent minerals, NiO content (0.3~0.4 wt%) and MnO content (0.1~0.2 wt%) of olivine are similar to those of mantle xenoliths worldwide, also indicating that studied spinel lherzolite xenoliths were mantle residues having experienced 20~25% partial melting. The geochemical and textural characteristics have close relations showing that LREE and incompatible trace elements content of orthopyroxene and clinopyroxene increases from protogranular through porphyroclastic to mylonitic. These observations suggest that the studied mantle xenoliths experienced metasomatism by LREE enriched melt or fluid after partial melting, indicating a close relation between deformation and metasomatism. The metasomatism was possibly confined to narrow shear zones from where porphyroclastic and mylonitic textured xenoliths originated. These shear zones might favorably drive the percolation of LREE-enriched melts/fluids responsible for the metasomatism in the lithospheric mantle below the Jeju Island.