• Analytical Science and Technology
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• v.19 no.5
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• pp.383-388
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• 2006

Simple post-wash method by ion chromatography (IC) was established for the rapid and precise determination of fluoride ion in wastewater from mine in fluorite mineralized area. High sulfate in sample was retained in a pre-column and less strongly held fluoride ion was transferred to the principal separation system using modified conventional IC with switching technique. An analytical column with high capacity (AS 9 HC) was used as a pre-column to retain the amount of high sulfate. A guard column (AG 14) as a separation column was used to increase the response of fluoride and reduce the system pressure. According to the recovery of fluoride ion with one detector and the observation of sulfate peak with another conductivity detector, the optimum switching time of 10-port chromatographic injector was 4.3 min. The limit of detection (S/N = 3) of fluoride in synthetic solution containing $500mg\;L^{-1}$ sulfate was $2.4{\mu}g/L$, with $25{\mu}L$ sample volume.

• Analytical Science and Technology
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• v.20 no.4
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• pp.323-330
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• 2007

A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.297-304
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• 2023

Domoic acid (DA), a neurotoxin produced naturally by diatoms, is responsible for incidents of amnesic shellfish poisoning. In this study, a modified analytical method was established to determine domoic acid in seafood using solid phase extraction cleanup and optimizing the amount of sample and extraction solvent to reduce interference effects. The modified method using high-performance liquid chromatography with ultraviolet detection was validated using three seafood matrices (mussel, red snow crab, and anchovy) at three concentrations (1, 2, and 4 mg/kg) and compared to the Food Code method. Compared to the Food Code method, the modified method showed better performance in terms of linearity (R²>0.999), detection limit (0.02-0.03 mg/kg), quantification limit (0.05-0.09 mg/kg), intra-/inter-day accuracy (86.2-100.4%), and intra-/inter-day precision (0.2-4.0%). Furthermore, the method was successfully applied for the analysis of 87 seafood samples marketed in Korea, and DA was detected at a low concentration of 140 ㎍/kg in one anchovy sample. These results suggest that the modified method can be used for routine determination of DA in seafood.

• Analytical Science and Technology
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• v.37 no.3
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• pp.143-154
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• 2024

In this study, we improved the vitamin C test method and reviewed data on the adjustable range of chromatography conditions for quantification. First, we adjusted the mobile phase conditions such as solvent composition, salt concentration, pH and column temperature and in particular, it was confirmed through an improved test method that the peak derived from the buffer solution could be clearly separated from the target component, vitamin C by adjusting the pH. The retention time of vitamin C was partially changed by adjusting the column diameter, length and particle size but the number of theoretical plates indicated similar values and did not affect the separation and quantitative analysis of the target component. The flow rate according to the column specifications was derived from the equation proposed by the U.S. FDA (Food and Drug administration) and the Korean MFDS (Ministry of Food and Drug Safety), and evaluation of the applicability to vitamin complexes showed high selectivity for vitamin C even with altered stationary phase conditions and flow rates. In conclusion, vitamin C can be optimally separated and detected by changing the chromatographic method conditions and it was confirmed that the mobile and stationary phase conditions of liquid chromatography can be slightly adjusted in case the assay method uses an isocratic elution.

• Analytical Science and Technology
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• v.24 no.5
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• pp.345-351
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• 2011

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

• Journal of the Korean Society of Food Science and Nutrition
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• v.45 no.1
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• pp.1-11
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• 2016

This study was conducted to investigate effect of the acetylcholinesterase inhibitor activity, the protective effect of the extract on SH-SY5Y cell death by $H_2O_2$, the memory improvement from scopolamine-induced rat. Moreover, the antioxidant activity of isorhamnetin from the dropwort (Oenanthe javanica) was investigated. Acetylcholinesterase inhibitor activity was highest (28.59%) in Hwasun O. javanica extract (H-OJE). H-OJE and Naju O. javanica extract (N-OJE) were not significantly different. SH-SY5Y cell death deceased to 37.23% and 36.68% for H-OJE and N-OJE, respectively, following treatment with the extracts. O. javanica extracts showed a protective effect against $H_2O_2$-induced neurotoxicity. Treatment with O. javanica extracts slightly improved scopolamine-induced (1 mg/kg, i.p.) memory impairment in rats. H-OJE contained the highest total phenolic and flavonoid contents of 117 mg/g and 30 mg gallic acid equivalents/g, respectively, and had a DPPH radical scavenging activity ($SC_{50}$) of $113.8{\mu}g/mL$ and ABTS radical scavenging activity of $48.2{\mu}g/mL$, which was higher than the other extracts. The thiobarbituric acid reactive substances value was highest (50.2%) in H-OJE. Antioxidant activity differed significantly among dropwort extracts. Isorhamnetin was known as one of the flavonoid and for having neuroprotective effect. So we analyzed acid-hydrolyzed O. javanica extract HPLC. The results were that peak at 14 min and spectrum of the extracts was consistent with standard solution. The results of LC/MS/MS analysis were that the extract and standard solution were confirmed total ion chromatogram at identical time, precursor ion was 317 $[M-H]^+$ m/z, product ion was 302 $[M-H]^+$ m/z. Overall, the results showed that the dropwort extract led to memory improvement and had antioxidant activity. Based on these finding, further research to investigate the production of ethanol extract of dropwort as a processed food is warranted.

• Korean Journal of Soil Science and Fertilizer
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• v.41 no.4
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• pp.260-266
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• 2008

Small lysimeter experiment under rain shelter plastic film house was conducted to investigate the effect of soil characteristics on the leaching and soil solution concentration of nitrate and phosphate. Three soils were obtained from different agricultural sites of Korea: Soil A (mesic family of Typic Dystrudepts), Soil B (mixed, mesic family of Typic Udifluvents), and Soil C (artificially disturbed soils under greenhouse). Organic-C contents were in the order of Soil C ($32.4g\;kg^{-1}$) > Soil B ($15.0g\;kg^{-1}$) > Soil A ($8.1g\;kg^{-1}$). Inorganic-N concentration also differed significantly among soils, decreasing in the order of Soil B > Soil C > Soil A. Degree of P saturation (DPS) of Soil C was 178%, about three and fifteen times of Soil B (38%) and Soil A (6%). Prior to treatment, soils in lysimeters (dia. 300 mm, soil length 450 mm) were tabilized by repeated drying and wetting procedures for two weeks. After urea at $150kg\;N\;ha^{-1}$ and $KH_2PO_4$ at $100kg\;P_2O_5\;ha^{-1}$ were applied on the surface of each soil, total volume of irrigation was 213 mm at seven occasions for 65 days. At 13, 25, 35, 37, and 65 days after treatment, soil solution was sampled using rhizosampler at 10, 20, and 30 cm depth and leachate was sampled by free drain out of lysimeter. The volume of leachate was the highest in Soil C, and followed by the order of Soils A and B, whereas the amount of leached nitrate had a reverse trend, i.e. Soil B > Soil A > Soil C. Soil A and B had a significant increase of the nitrate concentration of soil solution at depth of 10 cm after urea-N treatment, but Soil C did not. High nitrate mobility of Soil B, compared to other soils, is presumably due to relatively high clay content, which could induce high extraction of nitrate of soil matrix by anion exclusion effect and slow rate of water flow. Contrary to Soil B, high organic matter content of Soil C could be responsible for its low mobility of nitrate, inducing preferential flow by water-repellency and rapid immobilization of nitrate by a microbial community. Leached phosphate was detected in Soil C only, and continuously increased with increasing amount of leachate. The phosphate concentration of soil solution in Soil B was much lower than in Soil C, and Soil A was below detection limit ($0.01mg\;L^{-1}$), overall similar to the order of degree of P saturation of soils. Phosphate mobility, therefore, could be largely influenced by degree of P saturation of soils but connect with apparent leaching loss only more than any threshold of P accumulation.

• Analytical Science and Technology
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• v.25 no.1
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• pp.76-82
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• 2012

The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.202-208
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• 2012

A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.

• Applied Biological Chemistry
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• v.45 no.2
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• pp.101-107
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• 2002

The essential oils isolated from leaves, flowers, stems, and fruits of Vitex rotundifolia by steam distillation and extraction (SDE) method were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). A total of 76 components detected by GC, 42 components were identified positively by GC-MS and GC co-injection with authentic standards, and 34 components were identified tentatively by mass spectral data only. They included 16 monoterpene hydrocarbons, 30 oxygenated hydrocarbons, 10 sesquiterpene hydrocarbons, 8 oxygenated sesquiterpenes, 3 diterpenes, and 9 miscellaneous components. The major components in the oil from the leaves were ${\alpha}-pinene$ (30.25%), 1,8-cineole (19.89%), sabinene (9.56%), ${\alpha}-terpineol$ (7.94%), ${\beta}-pinene$ (5.69%), and terpinen-4-ol (2.37%), and those in the flower oil were ${\alpha}-pinene$ (25.47%), 1,8-cineole (7.69%), manoyl oxide (6.21%), ${\beta}-pinene$ (4.20%), ${\alpha}-te.pineol$ (3.76%), and sabinene (2.78%). The major components in the oil from the stems were ${\alpha}-pinene$ (13.24%), ${\alpha}-terpineol$ (10.64%), 1,8-cineole (4.40%), manoyl oxide (4.02%), ${\beta}-pinene$ (2.39%), and terpinen-4-ol (2.21%) while those in the oil from the fruits were ${\alpha}-pinene$ (20.24%), 1,8-cineole (11.47%), ${\beta}P-pinene$ (9.79%), ${\alpha}-terpineol$ (7.08%), sabinene (3.68%), and limonene (2.77%). The percentage composition of monoterpenes in the oils from the leaves and the fruits were higher than in those from the flowers and the stems, whereas the oil from the flowers and the stems were characterized by a large content of sesquiterpenes, diterpenes and other unknown high molecular weight components.