• Analytical Science and Technology
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• v.24 no.5
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• pp.352-359
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• 2011

An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

• Journal of Food Hygiene and Safety
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• v.22 no.4
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• pp.370-374
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• 2007

An analytical method for the simultaneous determination of four tetracycline (oxytetracycline, tetracycline, chlortetracycline, doxycycline) in egg samples was developed and validated using liquid chromatography with ultraviolet detection. Egg samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase C8 column with gradient elution using a mobile phase of 20 mM oxalic acid (pH 1.5)/acetonitrile. The procedure was validated according to the Food Drugs Administration guideline determining accuracy, precision, and limit of detection. Mean recovery of tetracyclines from spiked egg samples (50, 100, 200, 400, and $800{\mu}g/kg$) were 78.8-109.3%. Linearity in concentration range of $50-800{\mu}g/kg$ was obtained with the correlation coefficient $(r^2)$ of 0.994-0.999. The intra- and inter-day precision (relative standard deviation; RSD) was between 0.3-12.8 and 0.2-11.7%, respectively. Limit of detection (LOD) and limit of quantification (LOQ) for the investigated tetracyclines were 30 and $50{\mu}g/kg$ depending on egg samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of tetracycline residues in dairy egg.

• Korean Journal of Food Science and Technology
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• v.39 no.3
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• pp.246-254
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• 2007

Fresh tea leaves grown in Jeju Island and Jeonnam Province of South Korea were plucked and processed. Volatile compounds (VCs) were analyzed and identified with SPME-GC/GC-MS/GC-O. The VCs of green teas were classified into two major categories based on their aroma characteristics: the Greenish (Group I), and Floral (Group II) odorants. It was found that the VCs were decreased significantly in fresh tea leaves as they were plucked at the later stages of cultivation. The ratio of VCs responsible for Group I and Group II compounds was well-balanced in tea leaves plucked in May, but the balances were changed when the fresh leaves were processed. The major VCs of fresh tea leaves in Jeju and Jeonnam were n-hexanal, E-2-hexenal, Z-3-hexenal, myrcene, benzyl alcohol, linalool, and phenyl alcohol. Also, Jeju and Jeonnam tea leaves had different aroma composition. n-Heptanol, ${\beta}-pinene$, benzaldehyde, and ethyl salicylate were found in Jeju fresh tea leaves, and Z-3-hexenol, E-2-hexenol, and methyl n-heptanoate were detected in Jeju dry tea leaves. On the other hand, Z-linalool oxide and myrcene were found in Jeonnam dry tea leaves. The SPME-GC method showed high reproducibility (RSD, 7.4%) with no-artifact formation. In this study, optimum plucking period of tea leaves could be determined for production of high quality green tea with a well-balanced aroma and characteristic VCs in green tea according to growing areas.

• Journal of Korean Society of Environmental Engineers
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• v.28 no.6
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• pp.620-625
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• 2006

In this investigation, an ICP-DRC/MS method to measure arsenic with ultra-trace concentration without any interference by the compounds such as $^{40}Ar^{35}Cl^+\;and\;^{40}Ca^{35}Cl^+$, which disturb the precise measurement of arsonic was described. Thus, the oxgen was introduced into the dynamic reaction cell as reaction gas and reacted with arsenic ion created in plasma gas, $AsO^+$ was formed and detected with m/z of 91 by ICP-MS. It resulted in better detection limit than the old method with m/z of 75($As^+$). The optimum condition for oxygen supply as the reaction gas was 0.5 mL/min. The analytical features of the method are as follows: detection limit of $0.02{\mu}g/L$, precision(RSD) of 3.4%, and recovery of 96%. Arsenic in the water samples from the tributary streams to the Han River and the main stream of Paldang were analyzed with this method to identify the characteristics in its distribution. The concentration of As ranged from 0.53 to $1.26{\mu}g/L$. We could measure As with very low concentration, less than $1.0{\mu}g/L$, with excellent reproducibility. The method developed is expected to be applied to analyze As of the samples from sea water, food, and domestic and industrial waste water which have high concentration of Cl and/or Ca.

• Analytical Science and Technology
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• v.14 no.5
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• pp.432-441
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• 2001

An automated on-line portable preconcentration-short column gas chromatograph was developed, which used preconcentrator using adsorption tube with Tenax-GR and Curie-point heating. The developed system operated with 3 steps of processing, preconcentration, thermal desorption, and analysis and cleaning, and could continued operating within 1~2 min cycle. The recoveries of preconcentrator for toluene was ranged between $94.7{\pm}6.6%$ and $103.8{\pm}3.1%$ with less than 7% of RSD. For benzene, toluene and xylene(BTX) standard gas test, IDL was 41, 49, $472ng/m^3$ benzene, toluene and o-xylene, respectively. The BTX mixture was analyzed within 30 sec with baseline separation by the system equipped with 4 m long capillary column. The deficiency of separation power caused by short column was solved by the control of sample injection volume and inlet/outlet pressure ratio. The automated portable preconcentration-short column gas chromatograph system was found to be useful for the continuous air monitoring of BTX at ppb levels in ambient air.

• Analytical Science and Technology
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• v.11 no.5
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• pp.353-359
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• 1998

Danazol, one of the IOC banned substances, is a synthetic steroid which stimulates the synthesis of cellular protein with multiple and diverse biologic effects. To confirm the androgenic effects of danazol, levels of eight endogenous steroids and its major metabolite in human urine were simultaneously analyzed by selected ion monitoring (SIM) of GC/MS after oral administration. The recovery range of this method was 71.59%~93.56% and the RSD values of precision and accuracy test were 1.87%~10.48% and 1.32%~11.25%, respectively. The limits of detection of most of the drugs were $0.01{\sim}0.05{\mu}g/mL$ and calibration was carried out using urine spiked with each endogenous steroid and ethisterone standard at a concentration of 0.1, 0.5, 1.0, 10, 20 and $50{\mu}g/mL$ and with $10{\mu}g/mL$ of internal standard. Correlation coefficients varied between 0.963 and 0.991. The endogenous steroid profiling is one of valuatle tool for decteation of anabolic steroids.

• Journal of Ginseng Research
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• v.33 no.1
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• pp.8-12
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• 2009

A simple gradient HPLC method for rapid determination of major ginsenosides ($Rg_1$ and $Rb_1$) and unique ginsenoside (Rf) of Korean ginseng (Panax ginseng C.A. Meyer) was developed. Within 50min, three ginsenosides have been separated and identified on $\mu$-Bondapak $C_{18}$ column ($3.9{\times}300\;mm$, $10{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. The method was validated in terms of linearity, accuracy, and precision. The correlation coefficients ($r^2$) for calibration curves of ginsenosides were over 0.9997. The developed HPLC method was successfully applied to the analysis of ginseng samples and the recoveries of ginsenosides were in the range of $101.1{\sim}115%$ with RSD<3.2%. The developed method could be used for rapid evaluation of the ginsenosides $Rg_1$, $Rb_1$, and Rf.

• 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 the Korean Chemical Society
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• v.58 no.6
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• pp.535-542
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• 2014

A simple and efficient preconcentration method was developed using three-phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline). The tetracycline antibiotics were separated simultaneously on a column ($C_8$, $3.0{\times}150mm$, $3{\mu}m$) with high selectivity and sensitivity using gradient elution. Under optimized conditions (extraction solvent, heptanal; pH of donor, 9.0; pH of acceptor, 1.0; stirring speed, 700 rpm; NaCl salt, 0%; and extraction time, 60 min), enrichment factors (EF) were between 5.6 and 22.3. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of $0.08{\sim}0.8{\mu}g/mL$ and $0.4{\sim}1.6{\mu}g/mL$, respectively. The calibration curves were linear within the range of $0.1{\sim}32{\mu}g/mL$ with the square of the correlation coefficient being more than 0.995. The precision (as a relative standard deviation, RSD) and accuracy (as a relative recovery) within working range were 1.3~9.1% and 84~118%, respectively.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.1
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• pp.37-44
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• 2014

Preservatives such as paraben, phenoxyethanol, and chlorphene are commonly used in cosmetics thanks to cheap price and good antiseptic effect. Recently, consumers' concerns about their possible toxicity and skin irritation forced them to be replaced with straight 1,2-alkanediols. However, as the alkanediols may also irritate skin, limited amount of them should be used in cosmetics. Three 1,2-alkanediols including 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol in cosmetics were analyzed simultaneously by gas chromatogrphy with flame ionization detector. As a result of method validation, the specificity was confirmed by the calibration curves of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol showing good linearity correlation coefficient of above 0.999 over the concentration range of $100{\sim}1,200{\mu}g/g$. The limit of detection (LOD) and quantification (LOQ) of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol were 31, 40, and $19{\mu}g/g$ and 98, 108, and $57{\mu}g/g$, respectively. The precision (Repeatability) of the amount in cosmetics showed less than 2.0%. Relative Standard Deviation (% RSD) and the Accuracy (% recovery) of the amount in cosmetics showed 99.3 ~ 103.3, 99.4 ~ 106.7, 97.5 ~ 107.3% respectively. As a result, simultaneous analysis of antimicrobial three 1,2-alkanediols in cosmetics were possible. This method can be utilized in accurate quantitative analysis of 1,2-alkanediols in cosmetics.