• Analytical Science and Technology
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• v.22 no.4
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• pp.319-325
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• 2009

An effective and specific procedure for confirmation of neomycin, aminoglycoside antibiotic in honey was developed and validated. Honey was adjusted to pH 2 with 0.1M HCl and applied to weak cation-exchange SPE cartridge. Neomycin was eluted with basified methanol. Following separation by ion-pairing liquid chromatography, neomycin was analysed with positive electrospray ionization and MRM mode. Quantification was linear over the range of $5.0{\sim}250.0{\mu}g/kg$ ($r^2$ >0.9951). The precision (R.S.D.) and accuracy (as a bias) of quality control samples in honey ranged 11.5~18.7% and 10.9~20.9%, respectively. Established method can be applied to analysis of neomycin in honey.

• Horticultural Science & Technology
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• v.34 no.1
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• pp.183-194
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• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Clean Technology
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• v.25 no.4
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• pp.275-282
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• 2019

In this study, the extraction of Conger myriaster oil by using supercritical carbon dioxide (SC-CO₂) and organic solvent was investigated. The extraction conditions conducted for SC-CO₂ varied for pressure (25, 30 MPa) and temperature (45, 55 ℃), while the SC-CO₂ flow rate was kept constant during the experiment (27 g min^-1) and hexane was used as a conventional organic solvent. The extraction yield indicated that the best extraction condition would be SC-CO₂ at 55 ℃ and 30 MPa, resulting in the highest yield of 37.73 ± 0.14%. The oils were characterized for their fatty acid (FAs) composition using gas chromatography, while it was revealed that the major FAs were mystric acid, palmitoleic acid, oleic acid, electroosapentaenoic acid (EPA), and docosahexaenoic acid (DHA). The oxidation stability of the extracted C. myriaster oil was evaluated by measuring the acid value, peroxide value, and free fatty acid. The best oxidative stability was obtained from SC-CO₂ extracted oil at 30 MPa and 55 ℃. There was a significant difference in the color properties of the SC-CO₂ and hexane extracted oils, with the SC-CO₂ extracted oil showing better chromaticity than the oil extracted using hexane. Extracting oils from C. myriaster with SC-CO₂ could bring better economic benefits than using organic solvents. When supercritical carbon dioxide was used, there was no post-treatment process; thus, it was confirmed that this is a more environmentally friendly oil extraction method.

• Analytical Science and Technology
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• v.28 no.2
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• pp.125-131
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• 2015

A method was developed and fully validated for the determination of terbutaline, a β₂-receptor agonist, in human plasma. Plasma samples were prepared by solid-phase extraction with Sep-Pak silica, followed by high-performance liquid chromatography (HPLC). The terbutaline was pre-separated from the interfering components in plasma on a Luna C18 (2) column, and terbutaline and salbutamol as an internal standard were resolved and determined on a Luna Silica column. The two columns were connected by a switching valve equipped with silica pre-column. The pre-column was used to concentrate the terbutaline in the eluent from the C18 column before back-flushing onto the silica column with fluorescence detection at an excitation/emission wavelength of 276/306 nm. The method was shown to be specific by testing six different human plasma sources. Linearity was established for a concentration range of 0.4-20.0 ng/mL with a correlation coefficient of 0.9999. The lower limit of quantitation was 0.4 ng/mL with a precision of 10.1% as C.V.%.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2003.11a
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• pp.351-357
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• 2003

Transuranic elements such as Pu, Am and Cm in synthetic solution of spent nuclear fuel samples were determined by electrodeposition followed by alpha-spectrometry after separation using anion exchange and extraction chromatography in order to determine the transuranic elements in radwaste samples from nuclear power plants. Plutonium was separated by 12M HC1-0.1M HI as an eluent on anion exchange column. As a second step Am and Cm were separated in a group by DTPA-Lactic acid as the eluent on HDEHP coated column. The nuclides of $^{239}Pu$, $^{241}Am$및 $^{244}Cm$ separated were determined by alpha-spectrometry after electrodeposition in 0.1M $NaHSo_4$-0.53M $Na_2SO_4$buffer solution as an electrolyte. The recovery yields of $^{239}Pu$, $^{241}Am$및 $^{244}Cm$ were 83.8%, 85.2% and 86.3%, respectively, from the synthetic solution containing uranium and non-radioactive metal elements.

• Journal of Korean Society of Environmental Engineers
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• v.37 no.5
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• pp.293-302
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• 2015

Halonitromethanes (HNMs) are one of the most toxic groups of disinfection by-products. Recently, various studies have been fulfilled. An automated headspace-solid phase microextraction (SPME) gas chromatography/electron capture detector (GC-ECD) technique was developed for routine analysis of 9 HNMs in water samples. The optimization of the method is discussed. The limits of detection (LOD) and limits of quantification (LOQ) range from 90 ng/L to 260 ng/L and from 270 ng/L to 840 ng/L for 9 HNMs, respectively. Matrix effects in tap water and sea water were investigated and it was shown that the method is suitable for the analysis of trace levels of HNMs, in a wide range of waters. The method developed in the present study has the advantage of being rapid, simple and sensitive.

• Analytical Science and Technology
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• v.24 no.6
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• pp.421-428
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• 2011

In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

• Korean Journal of Food Science and Technology
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• v.52 no.1
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• pp.26-30
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• 2020

This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R²>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

• Korean Journal of Food Science and Technology
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• v.13 no.2
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• pp.107-113
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• 1981

Free sugars were isolated from ginseng root and its products and analyzed by using high performance liquid chromatogrphy. To isolate free sugars from aqueous sample solution fat-soluble components, crude saponin and protein were removed from the solution by extracting with benzene, water-saturated butanol and 80% ethanol, respectively. Free sugars found from both ginseng root and its products were fructose, glucose, sucrose and maltose, and the only sugar detected from red ginseng root and its products was rhamnose. Major sugar detected from fresh ginseng and white ginseng roots was sucrose, while sucrose and maltose were major sugars of red ginseng root.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.13 no.10
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• pp.4927-4935
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• 2012

Turmeric is a medicinal herb with various pharmacological activities. Curcumin, demethoxycurcumin(DMC) and bisdemethoxycurcumin(BDMC) were extracted from turmeric by dipping and ultrasonic wave method. And extraction efficiency was identified using solid phase extraction(SPE). The extracted sample were simultaneously separated and analyzed from three kinds of commercial $C_{18}$ reversed-phase high performance liquid chromatography using water and acetonitrile as mobile phase with isocratic elution mode. Flow rate 1.0mL/min, injection volume $10{\mu}L$ and column oven temperature $40^{\circ}C$ at 425nm wavelength has been conducted. From the experimental results, the optimum mobile phase composition of water/acetonitrile 50/50vol% using RS tech column. It is evident that the amount of curcuminoids extracted(extraction time 4h) by 100% MeOH was higher than any aqueous MeOH composition. Finally, in 100% water extraction, the amount(mAU${\times}$mim) of curcuminoids extracted by SPE was 14.3 and 24.5 times respectively higher than ultrasonic wave and dipping method. The shown results can be applied as sources for pharmaceuticals and functional material.