• The Korean Journal of Pesticide Science
• /
• v.4 no.1
• /
• pp.1-10
• /
• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• Journal of the Society of Cosmetic Scientists of Korea
• /
• v.40 no.4
• /
• pp.359-364
• /
• 2014

In this study, we developed a HPLC method for the separation and analysis of methylparaben and p-anisic acid, which are commonly used as a synthetic preservative and natural preservative, respectively. Methylparaben and p-anisic acid have same molecular weight (152.15 g/mol), similar structure and same maximum absorption wavelength (250 nm), thus they showed same retention time (RT) value (13.3 min) in HPLC experiment. We observed that two substances are separated on C18 column after methylparaben was derivatized selectively through the acetylation reaction. Instead, RT of the acetylated methylparaben was moved to 23.9 min from 13.3 min. The average retention time was $23.9{\pm}0.1min$ and peak area values was $5042882{\pm}4778$. In addition it showed a high linearity in the calibration curve with a correlation coefficient (R2) of 0.9999658. Detection and quantitation limits were $1.47{\mu}g/mL$ and $4.44{\mu}g/mL$, respectively. In conclusion, the developed method can be useful for separation and analysis of preservatives with similar structure in cosmetic fields.

• Journal of Ginseng Research
• /
• v.37 no.1
• /
• pp.135-141
• /
• 2013

A rapid, sensitive and selective analytical method was developed and validated for the determination of compound K, a major intestinal bacterial metabolite of ginsenosides in human plasma. Liquid-liquid extraction was used for sample preparation and analysis, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Compound K was analyzed on a Phenomenex Luna C18 column ($100{\times}2.00$ mm, 3 ${\mu}m$) with the mobile phase run isocratically with 10 mM ammonium acetate-methanol-acetonitrile (5:47.5:47.5, v/v/v) at a flow rate of 0.5 mL/min. The method was validated for accuracy (relative error <12.63%), precision (coefficient of variation <9.14%), linearity, and recovery. The assay was linear over the entire range of calibration standards i.e., a concentration range of 1 ng/mL to 1,000 ng/mL ($r^2$ >0.9968). The recoveries of compound K after liquid-liquid extraction at 1, 2, 400, and 800 ng/mL were $106.00{\pm}0.08%$, $103.50{\pm}0.19%$, $111.45{\pm}5.21%$, and $89.62{\pm}34.46%$ for intra-day and $85.40{\pm}0.08%$, $94.50{\pm}0.09%$, $112.50{\pm}5.21%$, and $95.87{\pm}34.46%$ for inter-day, respectively. The lower limit of quantification of the analytical method of compound K was 1 ng/mL in human plasma. The developed method was successfully applied to a pharmacokinetic study of compound K after oral administration in ten of healthy human subjects.

• Journal of Ginseng Research
• /
• v.42 no.2
• /
• pp.149-157
• /
• 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 IKEEE
• /
• v.20 no.4
• /
• pp.337-343
• /
• 2016

This study conducted the gamma ray spectroscopic analysis of the microcolumnar CsI:Tl deposited onto the SiPMs using thermal evaporation deposition. The SEM measured thickness of microcolumnar CsI:Tl and of its individual columns. From the SEM observation, the measured thickness of CsI:Tl were $450{\mu}m$ and $600{\mu}m$. The gamma ray spectroscopic properties of microcolumnar CsI:Tl, $450{\mu}m$ and $600{\mu}m$ thick deposited onto the SiPMs were analyzed using standard gamma ray sources $^{133}Ba$ and $^{137}Cs$. The spectroscopic analysis of microcolumnar CsI:Tl deposited onto the SiPMs included the measurements of response linearity over the $^{137}Cs$ gamma ray intensity; and gamma ray energy spectrum. Furthermore from the gamma ray spectrum measurement of $^{133}Ba$ and $^{137}Cs$, $450{\mu}m$ thick CsI:Tl showed good efficiency when measured with $^{133}Ba$ and $600{\mu}m$ thick CsI:Tl was highly efficient when measured with $^{137}Cs$.

• Journal of the Korean Chemical Society
• /
• v.61 no.2
• /
• pp.51-56
• /
• 2017

N-nitrosamines are the nitroso compounds which are produced by nitrosation reactions of the secondary amine and nitrite under acidic conditions. Approximately 300 species of N-nitrosamine have been tested for carcinogenicity in laboratory experiments, with 90% of them demonstrated carcinogenic effects different animal species, including higher primates. In 1978, IARC classified NDMA and NDEA as Group 2A, and NDPA, NDBA, NPIP, NPYR and NMOR as Group 2B. In this study, we established pretreatment and analytical method for N-nitrosamines (NDMA, NDEA, NMEA, NDPA, NDBA, NPIP, NPYR and NMOR) in human urine for biological monitoring of N-nitrosamines. The analytes were extracted using solid phase extraction (SPE), then quantitative analysis was performed by LC-(APCI)-MS/MS. The accuracies of the established method were between 85.8~108.7% and precisions were lower than 20%. The limit of detection (LOD) were between 0.0002 (NDBA) and 0.0793 (NDMA) ng/ml. The linearity obtained was satisfying for the 8 N-nitrosamines, with a coefficient of determination ($r^2$) higher than 0.999. The mean concentrations of N-nitrosamines in the urine were 2.645 mg/g creatinine for NDMA, 0.067 mg/g creatinine for NDEA, 0.009 mg/g creatinine for NMEA, 0.011 mg/g creatinine for NDBA, 0.271 mg/g creatinine for NPIP and 0.413 mg/g creatinine for NPYR. NDPA and NMOR were not detected. It can be used as a instrumental methodology for evaluation and risk assessment of human exposure to N-nitrosamines for the further research.

• Journal of the Korean Geophysical Society
• /
• v.3 no.3
• /
• pp.161-174
• /
• 2000

Bayesian inversion is a stable approach to infer the subsurface structure with the limited data from geophysical explorations. In geophysical inverse process, due to the finite and discrete characteristics of field data and modeling process, some uncertainties are inherent and therefore probabilistic approach to the geophysical inversion is required. Bayesian framework provides theoretical base for the confidency and uncertainty analysis for the inference. However, most of the Bayesian inversion require the integration process of high dimension, so massive calculations like a Monte Carlo integration is demanded to solve it. This method, though, seemed suitable to apply to the geophysical problems which have the characteristics of highly non-linearity, we are faced to meet the promptness and convenience in field process. In this study, by the Gaussian approximation for the observed data and a priori information, fast Bayesian inversion scheme is developed and applied to the model problem with electric well logging and dipole-dipole resistivity data. Each covariance matrices are induced by geostatistical method and optimization technique resulted in maximum a posteriori information. Especially a priori information is evaluated by the cross-validation technique. And the uncertainty analysis was performed to interpret the resistivity structure by simulation of a posteriori covariance matrix.

• Journal of Environmental Science International
• /
• v.18 no.10
• /
• pp.1135-1141
• /
• 2009

Carrots (Daucus carota L.) are consumed as an important dietary source of provitamin A including $\beta$-carotene, $\alpha$-carotene and lutein. An HPLC method was applied to determine the content of the carotenoid composition in carrot cutivars cultivated in Korea. HPLC analyses were carried out with five carrot cultivars (Socheon-5-chon, Hongsim-5-chon, Myeongju-5-chon, Seonhongbom-5-chon and Betarich) sown at April, 2007 and six cultivars (Yeoreum-5-chon, Hanyeoreum-5-chon, Sinheukjeon-5-chon, Bibariheukjeon, Manina and Betarich) sown at August of the same year. In general, the former varieties are not used for the sowing at summer because of their bolting (growth of floral axis). The former and the latter carrots were harvested after 110 and 96 days from seeding, respectively, and the carotenoids were extracted with acetone after freeze-drying. The amount of $\alpha$-carotene ($117.7{\sim}205.3\;{\mu}g/g{\cdot}DW$) was similar to that of $\beta$-carotene ($113.1{\sim}189.6\;{\mu}g/g{\cdot}DW$) for the carrot cultivars sown at spring, while the content ($46.2{\sim}71.1\;{\mu}g/g{\cdot}DW$) was about a half of $\beta$-carotene content ($92.5{\sim}140.2\;{\mu}g/g{\cdot}DW$) for the latter cultivars. In addition, the average content of lutein ($25.2\;{\mu}g/g{\cdot}DW$) in the former cultivars was eight times higher than that in the latter cultivars ($3.1\;{\mu}g/g{\cdot}DW$). Among the spring cultivation types, Socheon-5-chon and Myeongju-5-chon showed higher amount of $\alpha$-carotene and $\beta$-carotene, while the higher amount was determined in Yeoreum-5-chon and Sinheukjeon-5-chon among the autumn cultivation types. Validation of the HPLC-DAD method showed good linearity ($r^2$ > 0.997) of the three compounds analyzed in a wide concentration range ($0.025{\sim}20\;{\mu}g/ml$). The R.S.D. values for intra-day and inter-day precision were less than 19.2% and the mean recovery of each compound was 85.4~104.7%.

• The Korea Journal of Herbology
• /
• v.26 no.1
• /
• pp.41-46
• /
• 2011

Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.

• Journal of Physiology & Pathology in Korean Medicine
• /
• v.30 no.2
• /
• pp.88-94
• /
• 2016

The study was carried out to examine the anti-obesity effects of 40% ethanol extract from green tea seed (GS) and quantitative determination of caffeine as its major compound. The specificity was satisfied with retention time and UV spectrum by analysis of caffeine using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve with a coefficient of correlation (R²) of 0.9974. The amount of caffeine in GS was about 4.649 mg/g (0.465%) in the three times analysis, and relative standard deviation (RSD) was less than 0.452% by the validated method. The anti-obesity effects of GS were evaluated by using Oil Red O staining in 3T3-L1 adipocytes and body weight, visceral fat and lipid profiles in high fat diet (HFD)-induced C57BL/6 obese mice. Our results indicated that treatment with GS dose-dependently decreased lipid accumulation contents (p<0.001). Moreover, after oral administration for 30 days feeding with HFD-induced obses mice, GS (100 and 300 mg/kg/day) produced a significant decrease in serum total cholesterol (TC), glutamic oxaloacetic transaminase (GOT), glutamic pyruvic transaminase (GPT) and visceral fat. Thus, the result of this study indicate that the GS may be a useful resource for the management of obesity.