• Analytical Science and Technology
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• v.19 no.2
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• pp.149-154
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• 2006

A gas chromatography-mass spectrometric method was developed for the determination of formaldehyde in urine and saliva. In a 20 mL glass tube, 0.2 mL of urine or saliva was taken. Further, 1.8 mL of 0.1 M HCl, 0.1 mL of 2,000 mg/L 2,4-dinitrophenyl hydrazine and $20{\mu}l$ of 500 mg/L acetone-$d_6$ as internal standard were added in the tube and sealed tightly with cap. The solution was shaken for 20 min at room temperature and extracted using 4 mL of toluene. The extract was concentrated and redissolved with $100{\mu}l$ of acetonitrile, and then measured by gas chromatography-mass spectrometer (selected ion monitoring). The detection limit was 2.0 ng/mL and 0.5 ng/mL in saliva and urine, respectively. The calibration curves showed good linearity with r = 0.997 and 0.998 for saliva and urine, respectively. The method was used to analyze formaldehyde in rat urine after oral exposure. The developed method may be use ful to the monitoring for formaldehyde exposure in human.

• Analytical Science and Technology
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• v.22 no.3
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• pp.191-200
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• 2009

The aim of this study was to evaluate and establish of emission test method for liquid phase building materials such as paint, adhesive, sealant by emission cell. A small-scale emission chamber and emission cell were used to evaluate emission of TVOC from paint, adhesive, sealant. The quantity of TVOC emission were measured by a gas chromatography/mass spectrometry (GC/MS). Background concentration of TVOC was below $10{\mu}g/m^3$ in the emission chamber and cell. Air tightness and recovery in chamber and cell showed good results. The recovery of thermal desorber for toluene and n-dodecane were about 120%. The repeatability of response factor and retention time in GC/MS below 30%. The method detection limit of VOCs ranged 0.04~8.82 ng. The concentration of TVOC emission using emission cell was 1.35~1.41 times higher than emission chamber. The correlation of TVOC emission using chamber and cell method was significantly high (r=0.91~0.97).

• Asian Pacific Journal of Cancer Prevention
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• v.16 no.5
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• pp.2043-2049
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• 2015

Background: Serum Golgi protein 73 (GP73) as a novel and potential marker for diagnosing hepatocellular carcinoma (HCC) have been found to be elevated in HCC patients and associated with clinical variables representing tumor growth and invasiveness. The aim of this study was to prepare a pair of monoclonal antibodys (mAbs) against GP73 and develop a newly designed double-antibody sandwich enzyme-linked immunosorbent assay (s-ELISA), which would be used in the detection of serum GP73 (sGP73) as well as in the diagnosis of HCC. Materials and Methods: Produced by prokaryotic expression, the purified recombinant GP73 (rGP73), produced by prokaryotic expression, was used to immunize the Balb/c mice. Two hybridoma cell lines against GP73 were obtained by fusing mouse Sp2/0 myeloma cells with spleen cells from the immunized mice. The titers of anti-GP73 mAb reached 1:243,000. Western blotting analysis and Immunohistochemistry staining revealed that anti-GP73 mAb could recognize GP73 protein. The double-antibody s-ELISA was successfully established and validated by 119 HCC and 103 normal serum samples. Results: showed that the detection limit of this method could reach 1.56 ng/ml, and sGP73 levels in HCC group (mean=190.6 ng/ml) were much higher than those of in healthy controls (mean=70.92 ng/ml). Conclusions: Results of our study not only showed that sGP73 levels of HCC patients were significantly higher than those of healthy controls, but also indicated that the laboratory homemade anti-GP73 mAbs could be the optimal tool used in evaluating sGP73 levels, which would provide a solid foundation for subsequent clinical applications.

• Toxicological Research
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• v.24 no.1
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• pp.87-91
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• 2008

The present study was conducted to monitor the level of triflumizole residues in fruits (apple and pear) and vegetable (cucumber) samples in order to assess risk posed by the presence of such residues to the consumer. Triflumizole was applied at a recommended dose rate to apple and pear pulps and to a cucumber sample. The samples were collected at harvesting time following several treatments (three and/or four treatments). Triflumizole was extracted with methanol and re-extracted into dichloromethane. The presence of triflumizole was determined by HPLC with UV detection at 238 nm following the cleanup of the extract by open preparative chromatographic column with Florisil. The versatility of this method was evidenced by its excellent linearity (> 0.999) in the concentration range between 0.2 and 4.0 mg/kg. The mean recoveries evaluated from the untreated samples spiked at two different fortification levels. 0.1 and 0.4 mg/kg, and ranged from 87.5${\pm}$0.0 to 93.3${\pm}$2.6 for the tested fruits and vegetable, respectively, and the repeatability (as relative standard deviation) from three repetitive determinations of recoveries were no larger than 6%. The calculated limit of detection was 0.02 mg/kg and the minimum detectable level of 4 ng for triflumizole was easily detected. When triflumizole was sprayed onto the apple trees three times at 50-40-30 and 40-30-21 days prior to harvesting and four times onto the pear trees at 40-30-21-14 days prior to harvesting, the mean residual amounts of 0.05 and 0.06 mg/kg for apples and pears, respectively, were not detected in all of the treatments. When the cucumber sample was fumigated four times at 7, 5, 3 and 1 day prior to harvesting, the mean residual amount was not detectable. Triflumizole can be used safely when sprayed (wettable powder, 30% active ingredient) and fumigated (10%) 4 times at 14 and 1 day prior to harvesting to protect the fruits and vegetable, respectively.

• The Korean Journal of Nuclear Medicine Technology
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• v.13 no.3
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• pp.189-192
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• 2009

Purpose: Autopipetting system is an efficient automated equipment pipetting patient samples and reagents for rapid and accurate test. However, it can cause carryover between high concentration sample and low concentration sample. We evaluated carryover contamination of TECAN freedom Evo 100 autopipetting system. Materials and Method: We studied carryover contamination of $\alpha$-fetoprotein (AFP) and carcinoembryonic antigen (CEA) test on TECAN freedom Evo 100 autopipetting system. Very low concentration control samples were pipetted for comparison to the contaminated very low concentration samples. Then, The contaminated very low concentration samples were pipetted following the high concentration samples were pipetted alternately. The difference of low concentration samples represents carryover. The target value to decide carryover was 1ppm (parts per million). Results: For AFP, the mean values of the uncontaminated control samples and the contaminated samples were less than 0.6 IU/mL (the l imit of detection (LoD)). Carryover did not occur even though the high concentration sample which value was 650000 IU/mL. For CEA, the values of the low concentration control samples and the contaminated samples were less than 0.2 ng/mL (LoD). Carryover did not occur even though the high concentration sample which value was 65,000 ng/mL. Conclusions: Sample carryover was not found on TECAN freedom Evo 100 autopipetting system for AFP, CEA. However, carryover is a potential problem with automated instruments and robotic pipetting systems. Therefore, Clinical laboratories must periodically verify carryover contamination for the accurate and confidential test results.

• The Korean Journal of Pesticide Science
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• v.13 no.3
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• pp.133-147
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• 2009

In order to develop the simultaneous analytical method for pesticide residues which ones in soil are rapidly and inexpensively measured by, many analytical methods for individual pesticide residue and several methods for multi-pesticide residues in agricultural commodities and food were reviewed. Various gas chromatographic conditions and pre-treatment procedures were intensively investigated and modified. And then new optimum procedure was established and its proficiency was validated. The response on detectors of simultaneous determination of 180 pesticides out of pesticides used in Korea was tested. The number of pesticides that their limits of detection (LOD) equal or lower than $0.05\;mg\;kg^{-1}$ were 137 pesticides on ECD, 170 pesticides on NPD and 179 pesticides on ECD/NPD integrated. The retention times of most pesticides ranged appropriately between 10 minutes and 40 minutes in the proposed chromatographic conditions. But about 90 pesticides eluded between 20 minutes and 30 minutes and so they were not resolved enough. In partition with dichloromethane, ethyl acetate/hexane (1:1) and ethyl acetate, number of pesticides whose extraction efficiency ranged from 70% to 120%, were 163, 154 and 147, respectively.

• Journal of Pharmaceutical Investigation
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• v.36 no.5
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• pp.331-338
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• 2006

A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

• Environmental Engineering Research
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• v.18 no.4
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• pp.253-257
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• 2013

Exposure assessment for three major active ingredients used for humidifier disinfectants, polyhexamethylene guanidine (PHMG), oligo(2-(2-ethoxy)ethoxyethyl guanidinium chloride (PGH), and 5-chloro-2-methylisothiazol-3(2H)-one/2-methylisothiazol-3(2H)-one (CMIT/MIT) mixture, was conducted in a bedroom using an air sampler for a refined risk assessment. The experimental site was selected to reflect consumer exposure conditions. Aerosols formed by a humidifier were sampled during 8 hr at 7.5 L/min. Absorbed PHMG and PGH by the sampler were quantified using a spectrophotometric method, and high performance liquid chromatography-ultraviolet detection was used for CMIT/MIT. Three exposure scenarios were assumed for adding humidifier disinfectants to the humidifier water at 1, 2, and 10 times the volume recommended by the product suppliers, and the humidifier was on at its maximum rate of producing aerosols in order to consider reasonable worst-cases. The sampled mass of PHMG and PGH ranged 200 to $2,800{\mu}g$ and 140 to $1,900{\mu}g$, respectively, under different exposure conditions, whereas the absorbed mass of CMIT/MIT was barely detected at the detection limit of 0.11/0.29 mg/L, only at 10 times the recommended level. The resulting risk quotients for PHMG and PGH ranged 1,400 to 20,000 and 1,000 to 13,000, indicating that health risks could be significant. For CMIT/MIT mixture, risk quotients were much smaller than estimated by assuming that they are conservative in the indoor environment, probably due to oxidative reactions. The refined exposure assessment presented here may provide a useful tool for assessing risks posed by active ingredients in spray-type biocidal products.

• The Korean Journal of Pesticide Science
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• v.5 no.2
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• pp.1-12
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• 2001

A competitive indirect enzyme-linked immunosorbent assay (ci ELISA) for the organophosphorus insecticide acephate, O,S-dimethyl acetylphosphoramidothioate, was developed using a polyclonal antibody. Three different haptens mimicking the analyze and containing hexanoic acid moiety as a linker were synthesized, and then conjugated with the carrier proteins bovine serum albumin and keyhole limpet hemocyanin by the N-hydroxysuccinimide active ester method. Polyclonal antibodies raised against hapten-KLH conjugates in rabbits and the hapten-BSA conjugates as coating antigens were screened and selected for the assay in the homologous and/or heterologous ELISA system. The effects of various assay conditions, including blocking reagents, detergent content, organic solvents, pH, and preincubation of tile mixture of the polyclonal antibody and the analyze on the sensitivity were evaluated. The $IC_{50}$ value of acephate of 110 ng/mL was obtained in an optimized heterologous system using hapten-3-BSA as a coating antigen and a polyclonal antibody 8377, showing the detection range of 10-1000 ng/mL and the lowest detection limit of 4 ng/mL. The cross-reactivities of the structurally related insecticides, including methamidophos were less than 0.02%. These results indicate that the ELISA could be a convenient and alternative tool for monitoring acephate residues in agricultural products and environmental samples.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.83-88
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• 2017

We introduced disposable amperometric immunosensors for the detection of Sildenafil and Vardenafil (SDF/VDF) based on screen printed carbon electrodes. The developed immunosensors were used as a non-competitive sandwich-type enzyme immunoassay with a horseradish peroxidase label. The sensors were constructed on screen printed carbon electrodes by the simple electrochemical deposition of a reduced graphene oxide and chitosan (ErGO-CS) composite. To evaluate the sensing chemistry and optimize the sensor characteristics, a series of electrochemical experiments were carried out including electrochemical impedance spectroscopy, cyclic voltammetry and amperometry. The sensors showed a linear response to SDF/VDF concentrations in a range from 100 pg/mL to 300 ng/mL. The lower detection limit was calculated to be 55 pg/mL, the sensitivity was calculated to be $1.02{\mu}Ang/mL/cm^2$, and the sensor performance exhibited good reproducibility with a relative standard deviation (RSD) of 7.1%. The proposed sensing chemistry strategy and the sensor format can be used as a simple, cost-effective, and feasible method for the in-field analysis of SDF/VDF in functional or health supplement food samples.