• Journal of the Korea Academia-Industrial cooperation Society
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• v.18 no.12
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• pp.755-761
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• 2017

This study was conducted to establish an analytical method using an HPLC system equipped with a photodiode array (PDA) detector for the quality control of raw materials and cosmeceuticals containing fucoxanthin as an active ingredient. The column was octadecyl-functionalized silica gel and the measurement wavelength of the PDA was set to 499 nm. To validate the analytical method, the linearity of the calibration curve, detection limit, reproducibility and recovery rate were investigated and good results were obtained. The correlation coefficient of the calibration curve was 1.000 and the linearity was good in the concentration range of 0.5 ~ 100 ppm. Moreover, the limit of detection (LOD) was 0.1 ppm and the limit of quantification (LOQ) was 0.5 ppm. The results of the peak reproducibility test used for evaluating the system suitability showed that the RSD (n = 5) of the peak area was 2.0% and that of the retention time was 0.09%. In the spiking test, the recovery rate was $101.6{\pm}0.77%$. The fucoxanthin contents of the two kinds of fucoxanthin-containing raw materials were $49.6{\pm}3.3%$ and $1.03{\pm}0.016%$, respectively. In addition, the fucoxanthin content in the test product, which was intended to be 150 ppm, was $156.7{\pm}4.7ppm$. From the above results, it was concluded that this method could be applied to the quantitative analysis of fucoxanthin in cosmeceuticals.

• Analytical Science and Technology
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• v.15 no.5
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• pp.459-465
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• 2002

This study was performed to identify the proper analytical conditions of endotoxins regarding optical density in the workplace where metalworking fluids are used. This study found that "onset time method" was more accurate than "time to $V_{max}$ method". Reproducibility and accuracy analyzed by "onset time method" was greatly higher than the "time to $V_{max}$". The optical density of "0.03" was the most appropriate analytical condition among "onset time method". In this analytical condition, linearity of 0.998 was obtained and recovery rate ranged from 88% to 105% at the endotoxin concentrations below 5 EU/mL. No significant difference of endotoxins was observed between the optical densities of "0.03" and "0.05". However, correlation coefficients were different with statistical significance (p<0.01). This study confirmed that either the optical densities "0.03" or "0.05" should be used to analyze endotoxin. Of these optical density values, OD with correlation coefficient higher than 0.98 should be used to analyze endotoxin in environmental samples.

• Korean Journal of Food Science and Technology
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• v.42 no.5
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• pp.515-520
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• 2010

This research investigated benzimidazole residues (albendazole, fenbendazole, flubendazole, thiabendazole, oxibendazole) in livestock products. A total of 270 samples of livestock products (beef, pork and chicken) were purchased from local markets in Korea. Ethyl acetate was used to extract analytes from the sample, after which ethyl acetate extracts were purified using a MCX cartridge. Analytes were detected using liquid chromatography-tandem mass spectrometry. The limit of detection was 0.01-0.04 ppb, the limit of quantification was 0.03-0.13 ppb, the linearity ($r^2$) was 0.9992-1.0000, and the recovery was 70-85%. Residues of benzimidazoles, except for fenbendazole in pork, were not found in any of the 270 livestock samples. Fenbendazole was detected in the range of 1.2 to 3.1 ppb in 12 samples of pork.

• Analytical Science and Technology
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• v.29 no.6
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• pp.261-268
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• 2016

TXRF is a powerful technique for the soil sample analysis due to its ability to conduct quantitative analysis of powder sample without complicated pre-treatment processes. The conventional internal standard method used for this technique suffers from relatively low accuracy because of varying matrix effects of soil. In order to improve the accuracy, external standard method was applied to analyze two types of soil samples; acid-dissolutionized soil solution and detergent-suspended soil powder. Individual ICP-AES/MS grade standards were mixed, diluted and measured to create standard curves, but applying these curves for analyzing the soil solution sample did not make any improvement in comparison with the internal standard method. On the other hand, standard curves were created with using standard soil powders for the analysis of soil powder samples, and we found that this method increased the accuracy significantly relative to the internal standard method. Especially, Al, Fe, K, Ca, Ti, Ba, Mn, Sr, Rb, Cu was measured with relatively high accuracy (relative error = ${\pm}20%$).

• Journal of the Korean Chemical Society
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• v.39 no.12
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• pp.902-909
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• 1995

Detection limit as well as calibration curves on organophosphorus pesticide(dimethoate, diazinon, parathion-methyl, fenitrothion, malathion) and BHCs were measured for evaluation of utility on qualitative or quantitative analysis of pesticides with ion Trap mass spectrometer and quadrupole mass spectrometer. As ionization source, EI and CI were adopted for qualitative analysis of pesticides by comparison of each fragmentation pattern. At the same time, the utility as trace analysis techniques through scan or selected ion monitoring(SIM) mode was evaluated. With ion trap for all pesticides, detection limit(DL, 1 ${\mu}L$ injection) on scan mode was ranged 0.008∼0.225 ng at signal to noise ratio 3. With quadrupole DL on scan mode was ranged 0.23∼3.1 ng over 0.032∼0.68 ng on SIM mode. The calibration curve with ion trap generated good linearity over 0.99 as correlation coefficient. As clean up procedure, Bio Beads S-X3 was used for the separation of oils from five organophosphorous pesticides in flour extractant showing more than 80% as recovery at most cases. In case of BHCs in jinseng with Florisil column, the recovery of pesticides has been 60% to 90%.

• Journal of Food Hygiene and Safety
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• v.38 no.6
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• pp.420-429
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• 2023

GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.25 no.4
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• pp.81-96
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• 2020

Berthlot's reaction spectrophotometric method is generally used for the analysis of dissolved ammonium in seawater, but in recent years, a fluorescence method using an orthophthaldialdehyde-sulfite (OPA) fluorescent reagent is actively used internationally. In this study, we investigated the effects of the detection limit between the analysis methods, the reagent refractive index inherent in the spectrophotometric method, and the use of different calibration curves to understand the cause of the difference in dissolved ammonium concentration (about 0.31 𝜇M) observed in the seawater samples and a nutrient reference material between two institutions (KIOST (spectrophotometric method, one-order linear regression gradient only), Australia CSIRO (fluorescence method, quadratic formula)) conducted onboard the Australian R/V Investigator in 2017. The method detection limit (0.063 𝜇M) and the reagent refractive index background value (0.054 𝜇M) of the spectrophotometric method measured in this study could explain the difference in dissolved ammonium concentration values of the two institutes about 20% and 17%, respectively. However, when the concentration of the calibration curve of the spectrophotometric method was calculated using the same quadratic as the fluorescence method or the slope and intercept of linear regression, the difference in the dissolved ammonium concentration between the two institutions was reduced to less than the detection limit of the spectrophotometric method. Therefore, the difference in the concentration of dissolved ammonium between the two institutions, found in the nutrient reference materials and the seawater field sample during the international onboard nutrient inter-comparison experiment, may be attributed to be the effect of the different calibration curves used in the two methods rather than the effect of the difference in two analytical methods. When comparing the dissolved ammonium data from seawater samples in the future, it is recommended to pay attention to the information on the baseline, number of standard solutions, and calibration curve used in the analysis.

• Journal of the Korean Society of Food Science and Nutrition
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• v.46 no.2
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• pp.210-219
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• 2017

This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

• Journal of the Korean Chemical Society
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• v.38 no.12
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• pp.891-897
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• 1994

A method has been investigated for the determination of Selenium in Ginseng radix, Ganoderma Lucidum and Garlic using hydride generation atomic absorption spectrometry (HG-AAS). The effects of several acids and sodium tetrahydroborate concentration and their flow rate on the determination of Selenium for the hydride generation were investigated. The method of sample decomposition was also investigated using various mineral acids, such as nitric, perchloric and sulfuric acid in the closed system and foreign ion effects were studied. In the optimum conditions, we obtained calibration curve in the range 0-40 ppb. The analytical data of Garlic, Ganoderma Lucidum and Ginseng radix are 289, 296, 198 ppb, respectively.

• Analytical Science and Technology
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• v.10 no.2
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• pp.114-118
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• 1997

A stripping voltammetric scheme for the determination of osmium, based on the adsorptive accumulation of osmium in the presence of hydroxylamine, was described. Cyclic voltammetry was used to characterize the redox and interfacial processes. Optimal experimental conditions were found to be a stirred 0.05M hydroxylamine hydrochloride solution(pH 1.8), accumulation at -0.65V for 60s, and a differential pulse mode with a scan rate of 10mV/s. The detection limit was $6.3{\times}10^{-8}M$(12ppb) with the optimal condition.