• Bulletin of the Korean Chemical Society
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• v.32 no.12
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• pp.4265-4269
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• 2011

A method based on ethyl acetate extraction and gas chromatography with tandem mass spectrometry was developed for determining tetraconazole residues in fruits and vegetables. A 10 g homogenized sample was mixed with 10 mL ethyl acetate, shaken vigorously for 3 min, stored at $-20^{\circ}C$ for 15 min, and then vortexed vigorously for 1 min; 1 g NaCl and 4 g anhydrous $MgSO_4$ were added. The clean-up was carried out by applying dispersive solid-phase with 150 mg $MgSO_4$and 50 mg primary secondary amine. Three precursor product ion transitions for tetraconazole were measured and evaluated to provide the maximum degree of confidence. Average recoveries in fruits and vegetables at three levels (0.005, 0.05 and 0.5 mg/kg) ranged from 85.53% to 110.66% with relative standard deviations ($RSD_r$) from 1.3% to 17.5%. The LODs ranged from 0.002 to 0.004 ${\mu}g$/kg, and LOQs ranged from 0.006 to 0.012 ${\mu}g$/kg. This method was also applied to determine tetraconazole residue in cucumber dissipation experiment under field conditions. The half-lives of tetraconazole in cucumber were in the range of 2.1-3.1 days.

• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.639-644
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• 2011

A simple and highly sensitive chemiluminescence method to determine norfloxacin (NFLX) has been proposed by measuring the chemiluminescence (CL) intensities using a flow injection (FI) system. The CL intensity of the luminol-$H_2O_2$ system is strongly enhanced by the addition of Cu (II) in alkaline condition. The CL intensity is substantially increased after the injection of NFLX into the luminol-$H_2O_2$-Cu (II) system. The enhancement effect is attributed to a catalytic effect of Cu (II) due to the interaction with NFLX which forms a complex with the catalyst. Under the optimal conditions, the sensitizing effect of the CL intensity is proportional to the concentration of NFLX in the range of $1.5{\times}10^{-9}-5.9{\times}10^{-7}molL^{-1}$ (r = 0.9994) with a detection limit ($3{\sigma}$) of $2.98{\times}10^{-10}molL^{-1}$. The proposed method had good reproducibility with the relative standard deviation (RSD, n = 5) of 1.6% for $1{\times}10^{-7}molL^{-1}$ of NFLX. The possible reaction mechanism of the CL reaction is also discussed. This method has been successfully applied for the determination of trace amount of NFLX in pharmaceutical preparations and serum samples.

• Herbal Formula Science
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• v.20 no.2
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• pp.37-46
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• 2012

Objectives : Oyaksungi-san(Wuyaoshunqisan) has been used for treatment of stroke and rheumatoid arthritis in Korea. In this study, a simple and accurate high-performance liquid chromatography(HPLC) method was established for simultaneous determination of six main components, liquiritin, ferulic acid, naringin, hesperidin, neohesperidin, and glycyrrhizin in Oyaksungi-san, a traditional Korean herbal prescription. Methods : The analytical column for separation of six constituents was used a Gemini $C_{18}$ column maintained at $40^{\circ}C$. The mobile phase consisted of two solvent systems, 1.0% (v/v) acetic acid in $H_2O$ (A) and 1.0% (v/v) acetic acid in acetonitrile (B) by gradient flow. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 254 nm for glycyrrhizin, 280 nm for liquiritin, naringin, hesperidin, and neohesperidin, and 320 nm for ferulic acid. Results : Calibration curves were acquired with $r^2$ values ${\geq}0.9998$. The results of recovery test were 91.58%-105.90% with a relative standard deviations (RSDs, %) value less than 2.0%. The values of RSD for intra- and inter-day precision were 0.03%-1.72% and 0.03%-1.63%, respectively. The contents of the six compounds in Oyaksungi-san were 0.33-9.30 mg/g. Conclusions : The newly established HPLC method will be helpful to improve quality control of Oyaksungi-san.

• Journal of Korean Society for Atmospheric Environment
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• v.22 no.4
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• pp.468-476
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• 2006

Hazardous air pollutants (HAPs) have high toxicity and bioaccurnulation potentials into human body even inbsmall amount (levels of ng/$m^3$). As the levels of HAPs might be controversial, it has been become essential to establish the analysis method for correct results. In this study, various analysis methods of VOCs and Aldehydes were compared in order to select the proper methods in our condition. Sampling and analysis method of VOCs were followed to EPA TO-14a and TO-17. VOCs were collected in absorption tube and separated by thermal desorption unit then analyzed by GC/MSD. Aldehydes were sampled in DNPH-cartridge and extracted into solution then analyzed by HPLC as the same condition of EPA TO-13a. This study also shows the results of QA/QC system of selected methods. Some experiments could be improving the data assurance blank test, calibration check, repetition precision check, the determination of detection limit and reproducibility of the retention time. Precisions of VOCs and aldehydes were ranged in 2$\sim$9% and 1$\sim$4% RSD, respectively. Recovery rate of VOCs showed variable ranges from 60 to 133.5%. MDL of VOCs and aldehydes were 0.044$\sim$0.284 ppb and 0.14$\sim$1.02 ng, respectively.

• Environmental Engineering Research
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• v.25 no.4
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• pp.579-587
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• 2020

Novel silane grafted bentonite was obtained using the natural bentonite as precursor material. The material which is termed as nanocomposite was characterized by the Fourier Transform Infra-red (FT-IR) and X-ray diffraction (XRD) methods. The surface imaging and elemental mapping was performed using Scanning Electron Microscopic (SEM/EDX) technique. The electroanalytical studies were performed using the nanocomposite electrode. The electroactive surface area of nanocomposite electrode was significantly increased than the pristine bentonite or bare carbon paste based working electrode. The impedance spectroscopic studies were conducted to simulate the equivalent circuit and Nyquist plots were drawn for the carbon paste electrode and nanocomposite electrodes. A single step oxidation/reduction process occurred for As(III) having ΔE value 0.36 V at pH 2.0. The anodic stripping voltammetry was performed for concentration dependence studies of As(III) (0.5 to 20.0 ㎍/L) and reasonably a good linear relationship was obtained. The detection limit of the As(III) detection was calculated as 0.00360±0.00002 ㎍/L having with observed relative standard deviations (RSD) less than 4%. The presence of several cations and anions has not affected the detection of As(III) however, the presence of Cu(II) and Mn(II) affected the detection of As(III). The selectivity of As(III) was achieved using the Tlawng river water sample spiked with As(III).

• Analytical Science and Technology
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• v.15 no.5
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• pp.482-487
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• 2002

International Olympic Committee (IOC) prohibits the use of carteolol which is one of ${\beta}$-blockers. To prove whether carteolol product was taken or not, the analytical method in urine using GC/MS was established, and metabolism and excretion study were evaluated. As compared with acid hydrolysis, enzyme hydrolysis method was more efficiency. Coefficients of variation for intra-assay precision was around 10%. Error was less than 5% except the concentration of $0.05{\mu}g/m{\ell}$. Recovery was 78.5% at $2{\mu}g/m{\ell}$. Free carteolol, conjugated carteolol, and small amount of p-OH carteolol were found in dosed human urine samples. The conjugated form was being 59.4% of the total carteolol in human urine. The amount of carteolol renal excreted for 72 h after oral dose of 10 mg of carteolol was 49% of the administred dose.

• Analytical Science and Technology
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• v.8 no.1
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• pp.9-16
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• 1995

The low concentration of cadmium in the whole-blood was determined by graphite furnace atomic absorption spectrometry(GFAAS) after the sample was diluted five-fold by 1% Triton X-100, 2% $(NH_4)_2HPO_4$ as matrix modifier and pyrocoated graphite tube with L'vov platform was tried remove the interferences of blood matrix and reduce the loss of volatility of cadmium at higher ashing temperature($600^{\circ}C$). The criteria for evaluating the accuracy and precision of this analysis was confirmed by analysis of interlaboratory comparison(Japan) and NIST SRM No. 909(Cd in Serum). The limit of the determination for cadium was 0.1ng/ml and the relative standard deviation(RSD) at 1.0ng/ml level was about 10% for the GFAAS.

• Analytical Science and Technology
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• v.30 no.6
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• pp.379-389
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• 2017

In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

• Korean Journal of Pharmacognosy
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• v.43 no.2
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• pp.137-146
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• 2012

Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

• Korean Journal of Pharmacognosy
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• v.51 no.3
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• pp.217-221
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• 2020

Cirsium japonicum var. maackii (CM) has been used to treat certain medical conditions such as hemorrhage, hepatitis, and hypertension. Cirsimaritin was previously found as the major flavonoid in CM and is said to contribute to its pharmacological effects. There are currently no reports detailing the qualitative and quantitative detection of phytochemical indicators in the aerial parts of CM. Therefore, we developed a method to rapidly identify and quantify cirsimaritin in CM using HPLC/UV, and we optimized and validated this analytical method. The results showed good linearity in the concentration range tested (0.25-0.015 mg/mL, r² ≥ 0.9999), accuracy (93.9-111.3%), and precision (RSD ≤ 0.59%). The developed method can therefore be used for the rapid evaluation of cirsimaritin in CM.