• Biomolecules & Therapeutics
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• v.6 no.3
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• pp.289-295
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• 1998

The bioequivalence of two nilvadipine products was evaluated in 16 normal male volunteers (age 22-32 yr, body weight 57-80 kg) following sidle oral dose. Test product was Overca $l_{R}$ tablet (Choong-Wae Pharm. Corp., Korea) and reference product was Nivadi $l_{R}$ tablet (Hyundai Pharm. Corp., Korea). Both products contain 4 mg of nilvadipine. One tablet of the test or the reference product was administered to the volunteers, respectively, by randomized two period cross-over study (2$\times$2 Latin square method). The determination of nilvadipine was accomplished using a validated capillary column GC with electron-capture detection. As a result of the assay validation, the quantiflcation of nilvadipine in human plasma by this technique was possible down to 0.5 ng/ml using 1 ml of plasma. Absolute overall recovery from five replicate analyses of nilvadipine-spiked sample were 88.4$\pm$ 10.24% (mean$\pm$ 5.D.) for human plasma of 10 ng/ml. The coefficients of variation (C.V.) were less than 20% and the actual concentration of nilvadipine measured by GC ranged from 80 to 99% in all plasma. Average drug concentrations at each sampling time and pharmacokinetic parameters calculated were not significantly different between two products (p>0.05); the area under the curve from time zero to 8 hr (AUCo-$_{8 hr}$) (22.8$\pm$5.90 vs 22.2$\pm$6.10 ng . hr/ml), maximum plasma concentration ( $C_{max}$) (10.0$\pm$2.85 vs 9.3$\pm$3.28 ng/ml) and time to reach maximum plasma concentration ( $T_{max}$) (1.2$\pm$0.31 vs 1.3 $\pm$0.47 hr). The differences of mean AU $Co_{8hr}$ $C_{max}$, and $T_{max}$ between the two products (2.25, 7.65, and 10.30%, respectively) were less than 20%. The power (1-$\beta$) and treaeent difference (7) for AU $Co_{8hr}$, and $C_{max}$ were more than 0.8 and less than 0.2, respectively. Although the power for Tmax was under 0.8, Tm\ulcorner of the two products was not significantly different from each other (p>0. 05). These results suggest that the bioavailability of Overeat tablet is not significantly different from that of Nivadil tablet. Therefore, two products are bioequivalent based on the current results.sults.lts.lts.lts.

• Korean Chemical Engineering Research
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• v.56 no.6
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• pp.832-840
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• 2018

In this study, both of the concentration of benzo(a)pyrene in 5 species (total 50 samples) of medicinal herbs and their transfer ratios in the preparation steps of water extract(decoction) and soft extract, were measured by HPLC/FLD. The calibration curve of benzo(a)pyrene shows excellent correlation over the concentration range of 3~40 ng/mL with the correlation coefficient ($R^2$) of 1.000. The detected benzo(a)pyrene concentrations from the medicinal herbs ranged from non-detection to $37.54{\mu}g/kg$, and their average was $6.73{\mu}g/kg$. Among the total samples, 15 samples (i.e., 30%) exceeded the limit of herbal medicine benzo(a)pyrene criteria (i.e., $5{\mu}g/kg$) according to the notification No. 2009-302 from Ministry of Food and Drug Safety. In particular, the concentration of benzo(a)pyrene in Coptidis Rhizome was turned out to be the highest of $37.54{\mu}g/kg$. The detected benzo(a)pyrene concentrations from water extract(decoction), soft extract and remnant after boiling, ranged from non-detection to $2.31{\mu}g/kg$, non-detection to $2.28{\mu}g/kg$, and 2.18 to $21.91{\mu}g/kg$, respectively. In preparation of water extract(decoction) and soft extract, transferred benzo(a)pyrene was not detected or, if transferred, the maximal transfer ratios of benzo(a)pyrene were shown to be 8.9% and 9.8%, respectively. Therefore, the content of benzo(a)pyrene in the samples of herbal medicine used in this study, were reduced by more than 90% in preparation steps of water extract (decoction) and soft extract.

• Journal of Applied Biological Chemistry
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• v.65 no.1
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• pp.17-21
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• 2022

A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH₂) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r²) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

• Analytical Science and Technology
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• v.21 no.1
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• pp.34-40
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• 2008

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitative determination of lercanidipine in human plasma. After addition of internal standard (amlodipine), plasma was precipitated with acetonitrile and the supernatant was evaporated. The residues were dissolved in 50 % acetonitrile and analyzed by LC-MS/MS. Using MS/MS with multiple reaction monitoring(MRM) mode, lercanindipine were selectively detected without severe interference from human plasma. The standard calibration curve for lercanidipine was linear (r = 0.9994) over the concentration range 0.05-20.0 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of lercanidipine was lower than 11.7 % (correlation of variance, CV), and accuracy was between 94.4-114.8 %. This method has been successfully applied to the pharmacokinetic study of lercanidipine in human plasma.

• Analytical Science and Technology
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• v.22 no.5
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• pp.407-414
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• 2009

A simultaneous determination method for cholesterol, lanosterol and desmosterol was developed using gas chromatography/mass spectrometry. Urine was enzymatically hydrolyzed with ${\beta}$-glucuronidase/arylsulfatase. Samples were prepared using extractions with a mixture of ethyl acetate-hexane (2:3, v/v), followed by derivatization with a mixture of MSTFA/TMSI/TMCS (100:2:5 v/v/v). All analyses were performed using GC/MS in selective ion monitoring mode. Good linearities ($r^2=0.998{\sim}0.999$) in calibration curve and a satisfactory recovery (80.0%~113%) were achieved. Accuracy and precision values within ${\pm}15%$ in the concentration range of 5 to 200 ng/mL were also observed for all compounds. The developed method was applied to pravastatin-treated (70 and 250 mg/kg/day for 7 days, oral) hyperlipidemia rats. Those sterols were significantly lower in drug-treated rats compared to the controls, which justifies the drug efficacy. Therefore, these results indicate that the developed method was successfully applied to examine statin drug efficacy with urine sample.

• Journal of Bio-Environment Control
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• v.26 no.4
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• pp.235-241
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• 2017

This study was carried out to estimate growth characteristics of Kimchi cabbage cultivated in two different growing seasons and three transplanting dates in the greenhouses, and to create a predicting model for the production of Kimchi cabbage based on the growth parameters and climatic elements. Kimchi cabbages were transplanted three times at intervals of two weeks in spring and autumn growing seasons. Sigmoidal models for the estimation of fresh weight (Fw) was designed with days after transplanting, which were Fw=4451.5/[1+exp{-(DAT-34.1)/3.6}]($R^2=0.992$) and Fw=7182.0/[1+exp{-(DAT-53.8)/11.6}] ($R^2=0.979$), respectively. The relationship between fresh weight of Kimchi cabbage and growing degree days (GDD) was highly correlated, and the regression model represented by Fw=4451.5/[1+exp{-(GDD-34.1)/3.6}] ($R^2=0.992$) in spring growing season. The yield of Kimchi cabbage under spring and autumn growing season were estimated 11348.3kg/10a and 15128.2kg/10a, respectively, which were much different than outdoor culture each growing season, while greenhouse cultivation have shown similar results. To estimate the efficacy of prediction yield in Kimchi cabbage, we will need to supplement a predicting model, which was based on the parameters and climatic elements by the field cultivation.

• Analytical Science and Technology
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• v.31 no.4
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• pp.161-170
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• 2018

The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

• Analytical Science and Technology
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• v.29 no.2
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• pp.57-64
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• 2016

Many phthalic acid esters (PAEs), including DMP, DEP, DBP, BBP, and DEHP, as well as DEHA are widely used as plasticizers in plastics. An analytical method was developed and used to analyze these compounds at 41 industrial facilities. The coefficient of determination (R²) for each constructed curve was higher than 0.98. The method detection limit (MDL) values were 0.4–0.7 μg/L for PAEs and 0.6 μg/L for DEHA. In addition, the recovery rate was shown to be 77.0–92.3%, while the relative standard deviation was shown to be in the range of 5.8-10.5%. DMP (n = 3), DEP (n = 2), DBP (n = 2), BBP (n = 2), and DEHA (n = 3) were detected in the range of 2.2-11.1% in the influent. DEHP was a predominant compound and was detected at > MDL in both the influent (n = 16, 35.6%) and the effluent (n = 4, 10.0%) at a high removal efficiency (92–100%). The highest levels of residue in industrial wastewater influent were 137.4 μg/L of DEHP at plastic products manufacturing facility, 12.5 μg/L of DEHA at a chemical manufacturing facility, and 14.0 μg/L of DEP at an electronics facility. The highest concentration of effluent was 12.5 μg/L of DEHP at a chemical manufacturing facility, which indicated that the effluent was below the allowable concentration (800 μg/L). Therefore, the levels of PAEs and DEHA that are discharged into nearby streams could not influence the health of the ecosystem.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.2
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• pp.210-219
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• 2017

This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

• Journal of Veterinary Clinics
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• v.29 no.3
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• pp.233-236
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• 2012

Cefquinome, a fourth generation cephalosporin, has been solely used for veterinary medicine and has a broad antibacterial spectrum against gram-negatives and gram-positives being very stable to ${\beta}$-lactamases. This study was conducted to evaluate the bioequivalence of two cefquinome 2.5% products in piglets. Plasma cefquinome concentrations were analyzed by liquid chromatography-mass spectrometry (LC/MS). Mean maximum concentration ($C_{max}$) of test product ($Cequus^{(R)}$) and reference product ($Cobactan^{(R)}$) were $4.34{\pm}0.58$ and $4.22{\pm}0.47{\mu}g/mL$, and mean area under the concentration time curve ($AUC_{0{\rightarrow}{\infty}}$) values were $10.43{\pm}1.96$ and $10.25{\pm}2.98{\mu}g{\cdot}h/mL$, respectively. The 90% confidence intervals for the ratio of $C_{max}$ (0.941-1.115), and $AUC_{0{\rightarrow}{\infty}}$ (0.927-1.172) values for the test and reference products were within the acceptable bioequivalence limit of 0.80-1.25. It is concluded that two commercial cefquinome injectable solutions are bioequivalent in their extent of drug absorption in piglets.