• Analytical Science and Technology
• /
• v.20 no.5
• /
• pp.424-433
• /
• 2007

An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

• Natural Product Sciences
• /
• v.24 no.3
• /
• pp.199-205
• /
• 2018

To determine the optimum extraction conditions that give the highest yield of isoquercitrin and caffeic acid from Aster scaber, the effects of four extraction variables (solvent concentrations, extraction time, number of repeated extraction, and solvent volumes) on isoquercitrin and caffeic acid yield was examined via HPLC-UV. Our results showed that the highest extract and isoquercitrin yield were observed when A. scaber was extracted with 450 mL distilled water for 8 hr repeatedly for three times. In case of caffeic acid, the content was higher in the two repeated extracts. Also, content analysis of isoquercitrin in Aster species was performed in which A. fastigiatus, A. ageratoides, and A. scaber exhibited the highest isoquercitrin content at 6.39, 5.68, and 2.79 mg/g extract, respectively. In case of caffeic acid, the highest content of A. scaber and A. glehni was 0.64 and 0.56 mg/g extract, respectively. This study reports an optimized method for extraction of isoquercitrin and caffeic acid from A. scaber and evaluates potential sources of the compounds.

• Molecular Medicine Reports
• /
• v.19 no.3
• /
• pp.1809-1816
• /
• 2019

The extract of Sappan Lignum, the heartwood of Caesalpinia sappan L., has been used in medicine to improve blood circulation. Recently, the application of microwave extraction methods has been a major focus of research into the extraction of components from natural sources. In this experiment, we compared the anti-inflammatory effects of Sappan Lignum prepared by heat-70% EtOH extraction (CSE-H-70E) and microwave-70% EtOH extraction (CSE-MW-70E). High-performance liquid chromatography analysis was used to identify the compounds in these extracts. The heat-70% EtOH and microwave-70% EtOH extracts of Sappan Lignum had different chromatograms. CSE-MW-70E significantly inhibited the protein expression of iNOS and COX-2, PGE2, TNF-α, and reduced NO and IL-1β production in macrophages exposed to LPS, whereas, only high concentrations of CSE-H-70E (20 ㎍/ml) resulted in any effects. Furthermore, CSE-MW-70E upregulated heme oxygenase-1 (HO-1) expression. In addition, the use of tin protoporphyrin, an inhibitor of HO-1, confirmed the inhibitory effects of CSE-MW-70E on pro-inflammatory mediators. These results suggested that the CSE-MW-70E-mediated upregulation of HO-1 played an important role in the anti-inflammatory effects of macrophages. Therefore, these findings showed that microwave extraction can be utilized to improve the extraction efficiency and biological activity of Sappan Lignum.

• The Korea Journal of Herbology
• /
• v.29 no.6
• /
• pp.1-6
• /
• 2014

Objectives : This study was aimed to compare Gyejibokryeong-hwan (GBH) decoctions produced using different pressure levels for various extraction times to find the optimal extraction conditions through extraction yield, total soluble solids content (TSSC), hydrogen ion concentration (pH), and the contents of chemical compounds. Methods : Decoctions of GBH were prepared under the pressure levels of 0 or $1kgf/cm^2$ for 30-180 min using water as extraction solvent. The extraction yield, TSSC, and pH were measured, and the amounts of the chemical compounds were determined using high performance liquid chromatography-photodiode array detector. Results : The higher pressure and longer extraction time increased the values of TSSC and extraction yield, while decreased the pH value. The decoctions produced in 180 min by pressurized method and produced in 150 min by non-pressurized method showed maximum values of extraction yield and TSSC with minimum value of pH. The amounts of chemical compounds showed variations in pressurized and non-pressurized decoction during overall extraction times. The influences of pressure and extraction time on extraction yield, TSSC, pH, and the contents of chemical compounds were confirmed by regression analysis, which showed that all extraction values were significantly affected by at least one of two extraction factors, pressure and extraction time. Conclusions : This study suggests that the pressure and extraction time can significantly affect the extraction efficiency of components from GBH decoctions. However, optimal extraction conditions could not be chosen due to the variation of the amounts of chemical compounds.

• Bulletin of the Korean Chemical Society
• /
• v.20 no.6
• /
• pp.689-695
• /
• 1999

Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.3
• /
• pp.154-160
• /
• 2017

BACKGROUND:This study was carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiency was compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODS AND RESULTS:The BPs (bisphenol A, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range of MDLs by SPE and LLE methods was $0.0005{\sim}0.0234{\mu}g/L$ and $0.0037{\sim}0.2034{\mu}g/L$, and that of LOQs was $0.0015{\sim}0.0744{\mu}g/L$ and $0.0117{\sim}0.6477{\mu}g/L$, respectively. The calibration curve obtained from standard solution of $0.004{\sim}4.0{\mu}g/L$ (SPE) and $0.016{\sim}16{\mu}g/L$ (LLE) showed good linearity with $r^2$ value of 0.9969 over. Accuracy was 93.2~108% and 97.4~120%, and precision was 1.7~4.6% and 0.7~6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPA were highest among the BPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in the Yeongsan river basin. The concentration of BPB, BPC, BPE, BPF and BPS were not detected in all sites, whereas BPA was ranged $0.0095{\sim}0.2583{\mu}g/L$, which was $0.0166{\sim}0.0810{\mu}g/L$ for mainstreams, $0.0095{\sim}0.2583{\mu}g/L$ for tributaries, $0.0352{\sim}0.1217{\mu}g/L$ for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS. We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.

• Archives of Pharmacal Research
• /
• v.17 no.4
• /
• pp.244-248
• /
• 1994

A stereoselective and sensitive high performance liquid chromatography using fluoresecence deterctor was examined for the determination of R(-) and S(+)-salbutamol in human plasma. Solid phase extraction method using silica as sorbent was used to extract salbutamol racemates from the plasma matrices. After fractionation and freeze-drying of the eluates containing salbutamol racemates, they were separated and quantified on a chirla stationary column. The detection limit of each enantiomer was 2 ng/ml in human plasma (S/N=3).

• Bulletin of the Korean Chemical Society
• /
• v.18 no.12
• /
• pp.1256-1260
• /
• 1997

A series of acyclic polyethers bearing amide end-groups and lipophilic alkyl chains (3-5) were successfully synthesized with quantitative yields. Based upon the transport experiment in a bulk liquid membrane (BLM) system and solvent extraction, a very high selectivity of Pb2+ over other transition metal cations was observed. Measurement of thermodynamic parameters for complexation in methanol at 25 ℃ gave a strong evidence for excellent selective complexation for lead ion over other transition metal ions.

• Proceedings of the PSK Conference
• /
• 2003.04a
• /
• pp.290.1-290.1
• /
• 2003

Oxidative DNA damage has been associated with many disease. Quantation of DNA adducts is considered to be a useful biomarker of oxidative DNA damage because its formation can also be induced by oxidative stress. Extensive efforts have been taken to identify the analytical methods for minimizing the artifactual formation of oxidative DNA damage. We have done direct analysis of DNA adducts using LC/ESI-MS without urine sample extraction. (omitted)

• Fashion & Textile Research Journal
• /
• v.11 no.2
• /
• pp.337-343
• /
• 2009

This study systematically investigated a method for extraction of safflower (Carthamus tinctorius Linnaeus) colorants by ultrasonic treatment. Compared to pigments productivity and cell wall structures of safflower after general and ultrasonic method, the ultrasonic method showed high extraction efficiency of safflower pigments due to destruction of safflower cell wall caused by high vibration energies. Microscopic analysis confirmed the hypothesis that the ultrasonic treatment of safflower caused its cell wall structure loosened and made efficient extraction of safflower pigments. And also, LC-MS/MS analysis revealed that productivities of the yellow and red safflower pigments by ultrasonic method were 21.9% and 14.6% higher, respectively, than those of pigments extracted by general method. The ultrasonic extracted yellow and red colorants could be used to dye not only natural fibers like cotton, silk and wool, but also synthetic fiber like nylon, and generally gave a better color tone than the general extracted colorants from safflower due to the affinities of red and yellow colorant on different fibers. As the yellow and red colorant were extracted by ultrasonic treatment in water, the K/S value on of 550/440nm of cotton and rayon was increased but in the case of silk and wool the change of this value was almost not detected. Finally, this technique might provide a solution to establish reproducibility and standardization for the extraction and dyeing methods on fabrics.