• Analytical Science and Technology
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• v.16 no.2
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• pp.102-109
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• 2003

Microwave digestion and solid-state extraction were studied for determination of trace aluminum{Al(III)} in human urine samples. A mixed acid of nitric acid and hydrogen peroxide was added to urine samples, organic materials were destructed in a home microwave oven and dried in a drying oven. The dried residues were dissolved in a sulfuric acid solution. The solution was eluted through a XAD-4 resin column adsorbed with 8-hydroxyquinoline(Oxine, HQ). Al(III)-8-hydroxyquinolinate complex was formed in the column and eluted with 0.5 M nitric acid solution. The Al(III) eluted was determined by graphite atomic absorption spectrophotometry. Various experimental conditions of followings were investigated for the optimization : the type of acid to dissolve the residues, the amount of HQ adsorbed on the resin, the pH of sample solutions, the type and concentration of acid to elute the complex from column and so on. The contents of Al(III) in real samples were determinated by a calibration curve method. The recovery in standard spiked samples was 94~101% and the detection limit of this procedure was 0.05 ng/mL.

• Analytical Science and Technology
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• v.11 no.5
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• pp.374-385
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• 1998

Phytoestrogens are biologically active compounds derived from plants foods. It had been suggested that phytoestrogens, by inhibiting aromatase in peripheral and/or cancer cells and lowering estrogen levels, may play a protective role as antipromotional compounds during growth of estrogen-dependent cancers. Therefore, simultaneous analysis of estrogens and phytoestrogens is necessary to elucidate the possible involvement of phytoestrogens in estrogen metabolism. In this view, we developed a simple and reproducible procedure to quantitatively determine estrogen and phytoestrogen metabolites. The proposed method consisted of solid phase extraction using preconditioned Serdolit AD-2 resin, enzyme hydrolysis with ${\beta}$-glucuronidase/arylsulfatase from Helix pomatia, liquid-liquid extraction and TMS-ether derivatization. And the final determination was carried out by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode (SIM). The precision and accuracy of this method was evaluated through within-a-day and day-to-day test. Recovery range and detection limit were 71.96~105.66%, 2~4 ng/mL, respectively. Using this method, 17 estrogen and 5 phytoestrogen compositions in urine of normal subjects were analyzed. It was found that amounts and relative distribution of urinary phytoestrigens and estrogens showed different pattern in male and female subjects.

• Analytical Science and Technology
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• v.26 no.2
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• pp.135-141
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• 2013

The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.

• Journal of fish pathology
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• v.25 no.2
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• pp.95-101
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• 2012

The residue levels of sulfadimethoxine (SDM) was studied after oral administration to cultured olive flounder, Paralichthys olivaceus at $20{\pm}1.0^{\circ}C$. The concentrations of SDM in the plasma and liver were determined by HPLC-UV detector after a single dosage of 400 mg/kg body weight. The average recoveries of SDM in spiked samples between 2~50 ppm were 92.24~93.62% for plasma and 88.34~91.90% for liver. Limit of detection for SDM was 0.05 ppm by using this method. Samples were taken at 1 h, 6 h, 12 h, 24 h, 48 h, 72 h, 168 h, 240 h, 336 h and 480 h post-dose. The peak plasma and liver concentrations of SDM, which attained at 1 h post-dose, was $402.64{\pm}59.66{\mu}g/ml$ and $238.18{\pm}54{\mu}g/g$, respectively. Thereafter, it's elimination from both tissues was considerably faster following process of time. Their concentrations of SDM were not measurable at 480 h post-dose. Based on this results, dosage and withdrawal times for SDM could be used when it is prescribed with SDM in olive flounder.

• Journal of Food Hygiene and Safety
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• v.18 no.3
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• pp.95-100
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• 2003

Competitive direct enzyme-linked immunosorbent assay(cdELISA) of aflatoxin $B_1$ ($AFB_1$) in deonjang(Korean-style soybean paste) and kochujang(fermented hot peppersoybean paste) and the level of $AFB_1$ in modern or traditional style deonjang and gochujang, produced in Korea, was surveyed by cdELISA. From the standard curve of the cdELISA, the detection limit of $AFB_1$ was 0.2 ng/m/. The average recovery of $AFB_1$ was 71.5% in the range of 1~100 ng/g after spiking $AFB_1$ into deonjang and it means that it could be possible to detect the $AFB_1$ in these range by the cdELISA in deonjang. Among the 30 kochujangs tested, no $AFB_1$ was detected in kochujangs. Among the 30 deonjangs, $AFB_1$ was detected in 6 ones in the range of 1.0~6.0 ng/g. The occurrence of $AFB_1$ in deonjang and kochujang tested in this study was less than the Korea Standard and Specification of aflatoxin in foods (10 ppb).

• Journal of Food Hygiene and Safety
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• v.35 no.4
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• pp.312-318
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• 2020

A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH₂ solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.

• Journal of Life Science
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• v.16 no.6
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• pp.1006-1013
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• 2006

To High Throughput Screening (HTS), a homogeneous fluorescence polarization immunoassay (FPIA) was developed for the quantitative determination of ochratoxin A(OTA) using a $Victor^3$ (PerkinElmer). The homologous tracer, fluorescein-labelled OTA-EDF were synthesized and a specific OTA antibody has been used in the development of the method. It allowed the determination of OTA in the concentration range 0.5-200 ng/ml, with the detection limit of 0.3 ng/ml. The method developed was highly specific and reproducible. OTA spikes in unpolished rice extracts were determinable by FPIA with good recovery. For naturally contaminated unpolished rice samples some disagreement was observed between the results obtained by FPIA and HPLC, which could be related to the a little matrix effect observed for FPIA. Further research is needed to validate the procedure. On the basis of these initial results, this FPIA appears to meet the performance criteria for OTA screening of food samples without a complicated clean-up.

• Applied Biological Chemistry
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• v.45 no.3
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• pp.152-156
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• 2002

Soils near abandoned zinc mines were known to be contaminated with arsenic-rich mining by-products. To examine the potential impacts of arsenic- contaminated soils on plant growth, surface soils were subjected to sequential extraction. Results revealed that 54% and 74% total As and 74% total extractable As were bound to iron hydrous oxide, and water soluble fraction was below detection limit. Arsenic faction extracted using the Koran standard method(dissolution of metals via treatment of 1 N HCI) was strongly correlated with the Fe-bound As fraction ($r^2=0.884**$). Arsenic level in rice plant roots was the highest with a maximum value of 154.9 mg/kg, whereas it was below 0.6 mg/kg in grains. Arsenic level in rice plant roots was strongly correlated with those of Al-bound As ($r^2=0.821**$) and 1N HCI-extractable As levels ($r^2=0.801**$).

• The Journal of the Petrological Society of Korea
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• v.24 no.2
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• pp.77-90
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• 2015

The fission track registration techniques for accurate determinations of uranium in solid- and liquid-state geological materials were recommended and their applicability were examined. The determination of uranium can be achieved by optical counting of neutron-induced fission tracks of $^{235}U$ registered on solid-state track detectors under high magnification. In a dry registration method using powdered pellets of rocks (e.g., granite and coal) showing good uranium-affinity, it was not easy to decide an overall mean concentration over the total sample owing to track-clusters caused by frequent presence of uranium-bearing minerals. Separate scanning for homogeneous and track-clustered parts may be an alternative choice. Assuring the homogeneity over the whole sample, high reproducibilities were confirmed both from duplicate detections using mica and Lexan polycarbonate detectors and from multiple measurements at different thermal neutron fluences. The wet registration method using sealed quartz tubes is recommended to overcome the common heterogeneity in uranium concentrations of $10^1ppm$ and more. Adopting the wet registration, the uranium homogeneity was recovered below the $10^0ppm$ level and the lower detection limit was proved to reach without difficulty the $10^2ppb$ (i.e. $ng\;g^{-1}$) level.

• KSBB Journal
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• v.21 no.3
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• pp.212-219
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• 2006

The purpose of this study was to develop a assay system of host cell-derived residual proteins in final pharmaceutical products. Accurate and simple assay system for host cell-derived proteins(HCPs) is very important test item in pharmaceutical qualification control. In this study, methods for quantification of residual HCPs in recombinant anti-GPIIbIIIa antibody were developed using a process-specific immunoligand assay which was based on the Enzyme linked Immunosorbent assay(ELISA) system. The assay had a detection limit of 10.8 ng/ml of HCPs with a product concentration of 1 mg/ml. The practical implication of these results is that the developed ELISA system can be used for HCPs qualification control and this system will be applicable to develop another ELISA system of different antibody drug.