• Analytical Science and Technology
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• v.18 no.1
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• pp.43-50
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• 2005

A number of carbonyl compounds including formaldehyde and acetaldehyde are well known for their toxicity and irritancy. Hence, acquisition of both qualitative and quantitative tool for their analysis is essential to resolve issues associated with malodor or indoor pollution. Using HPLC/UV method, we examined various aspects involved in the measurements of formaldehyde in environmental samples. The results of our analysis indicated that its detection was made as low as 0.5 ppb (assuming 5 L of sample volume), while its precision was maintained near 2% in terms of relative standard error (RSE). When the stability of calibration was checked by variability of slope values obtained over long-term period (e.g., one month), its values were found to remain constantly with RSE values of 3%. It was also found that liquid-phase reaction between formaldehyde and DNPH proceed very slowly to attain equilibrium (one and half hour), while requiring adequate amount of DNPH to form their derivatives. The overall results of our study thus suggest that there are a number of factors to consider for the accurate analysis of formaldehyde in ambient air.

• 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.

• The Korean Journal of Pesticide Science
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• v.4 no.1
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• pp.1-10
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• 2000

The purpose of this study is to establish the assessment techniques of hazardous chemicals by the development of analytical method of biological samples. In this study, we have developed an extraction method of nine pesticides used for rice paddy that resulted in high recovery from the spiked human urine by the liquid-liquid extraction with diethyl ether at pH 7.0. Calibration curve obtained from each pesticide standard using by gas chromatography/mass spectrometry/selected ion monitoring has shown good linearity and detection limits were the range of $0.4{\sim}2.0$ ng/mL in urine. As a biological monitoring, urine samples of local farmers exposed directly to nine pesticides in the field were collected and analyzed by GC/MS. Of the tested pesticides, metabolites of phenthoate assumed were identified by GC/MS analysis. No parent compound was detected.

• The Korean Journal of Pesticide Science
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• v.18 no.4
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• pp.296-313
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• 2014

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.

• Journal of Food Hygiene and Safety
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• v.31 no.6
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• pp.432-438
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• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

• Analytical Science and Technology
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• v.28 no.5
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• pp.309-316
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• 2015

The analytical method of lead in plasma by ICP-MS was validated after securing environment within class 1,000 classification. We tested specificity and accuracy of within-run and between-run. According to measurement of the amount of suspended particulates in a clean room, 0.3~62 particles were detected in 0.3 µm size while 0.0~28.3 particles were observed in 0.5 µm size. Total suspended particulates met required environment with up to 90.3 particles. The MDL (Method detection limit) of the sample which has been fabricated using fetal bovine serum (FBS) blank was 1.77 ng/L, and LOQ (Limit of quantification) was 5.55 ng/L. The slope, intercept and correlation coefficient of the calibration curve were y=1.09×10⁻³x+4.88×10⁻² and r=0.9999, which showed good correlation. The specificity, within-run and between-run accuracy satisfied the standard at more than 50 ng/L. The average lead concentration in plasma of the general people, current workers and retired workers was 55.4 ng/L, 440 ng/L, and 132 ng/L.

• Analytical Science and Technology
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• v.23 no.1
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• pp.68-73
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• 2010

In order to develop the square wave voltammetric method determining cimetidine in an ampoule for injection, $5.00{\times}10^{-4}\;M$ cimetidine HCl solutions prepared with phosphate buffers of various pH values (3.01~8.97) were investigated by SWV. The well defined single peak due to the electrochemical reduction of -C=N-C$\equiv$N- in the structure of cimetidine moved towards the cathodic direction by -0.051V/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curves of cimetidine HCl in the concentration range between $1.00{\times}10^{-5}\;M$ and $5.00{\times}10^{-3}\;M$ prepared using three phosphate buffers yielded the slopes of 127,407nA/M (pH 3.01), 115,125nA/M (pH 5.00) and 111,287nA/M(pH 7.00) with excellent linearities of $R^2{\geqq}0.9997$. When one ampoule of Tagma Inj.$^{(R)}$ was analyzed by standard addition method by SWV, the within-day precision study (n=4) on the day of sample preparation resulted in the contents of cimetidine as $203{\pm}3.8\;mg$ (102% of the specified contents, RSD of 1.9%) and the inter-day precision (n=4) through 5 days was reasonable as 1.3% of RSD.

• Analytical Science and Technology
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• v.24 no.2
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• pp.119-126
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• 2011

Abstract: The amount of benzene, toluene, ethylbenzene, and o-xylene (BTEX) in 30 kinds of bottled waters purchased from market and 9 kinds of tap waters from home were determined using headspace solid phase microextraction (HS-SPME). The sample was stirred at 1200 RPM G for 4 min using a magnetic bar with $100\;{\mu}m$ PDMS as adsorbent for BTEX. Then it was desorbed from the fiber for 1 min at room temperature. Quantitation was achieved using standard calibration method. The limit of detection was determined as benzene 0.39 (${\pm}0.04$) ng/mL, toluene 0.08 (${\pm}0.04$) ng/mL, ethylbenzene 0.04 (${\pm}0.01$) ng/mL, and o-xylene 0.05 (${\pm}0.02$) ng/mL. Benzene and o-xylene were not detected in any samples, but toluene was detected in 11 samples, and ethylbenzene was detected just in 3 samples among 30 investigated bottled waters. The concentration range of investigated materials for toluene and o-xylene were $0.24({\pm}0.09)\sim2.95\;({\pm}0.08)\;ng/mL$, $0.08({\pm}0.06)\sim0.93({\pm}0.10)\;ng/mL$, respectively.

• Food Science and Preservation
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• v.22 no.4
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• pp.559-566
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• 2015

The aim of this study was to develop an analytical method for determination of T-2 toxin and HT-2 toxin level in cereals and to survey their levels using LC-MS/MS. The T-2 and HT-2 toxins were simultaneously analyzed by electrospray ionization with a positive ion mode and multiple reaction monitoring (MRM) after filteration and immuno-affinity column clean-up. A matrix-matched standard calibration used for quantification and recoveries of T-2 and HT-3 toxins were in the range of $100.6{\pm}7.2%$ and $96.8{\pm}9.4%$, respectively. Limits of detection and quantification of T-2 and HT-2 toxins were estimated to be 0.5 and $1.5{\mu}g/kg$, respectively. Each repeatability (RSRr) of T-2 and HT-2 toxins was determined to be 0.9~6.0%, and 4.9~6.1%, respectively. Total 115 samples cereals were collected from 9 types of cereals for analysis. The positive percentages of T-2 and HT-2 toxins obtained from collected samples were found to be 72% and 80%, respectively. The contamination level of T-2 toxin and HT-2 toxin in cereals were $37.1{\mu}g/kg$, and $5.4{\mu}g/kg$, respectively. Therefore, this study suggests that the developed method could be an useful analytical method to determine the T-2 and HT-2 toxin level in cereals and the present data could be used as a reference to estimate the risk assessment.

• Journal of the Korean Chemical Society
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• v.25 no.4
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• pp.275-282
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• 1981

A simple semiquantitative procedure was developed for the determination of sub-ppm level of chromium(VI) in aquatic samples by using an analytical micro-column packed with diphenylcarbazide(DPC) gel beads. DPC gel beads were prepared by swelling XAD-2 resin(115∼150 mesh in dry condition) in ethanol for 10min, packing into a glass column(1.5 mm bore, 65nm length) and adsorbing 1ml of ethanol solution of $2{\times}10^{-3}M$ DPC for 20min at room temperature. When 0.5ml of ethanol solution containing chromium(VI) was passed through the DPC gel column for 40min, the original white color of the reagent gel turned to red-violet from the up-stream of the column. As the length of colored band was proportional to the total amount of chromium(VI) in the sample solution passed through the column, the concentration of chromium(VI) could be determined from the calibration line which had been prepared by using the standard solution. Chromium(VI) ion as small as from 0.1 to 0.8 ppm could be determined with ${\pm}5{\sim}{\pm}15{\%}$ relative errors. Since other interfering cations were few, 100-fold excess of Fe(III), 50-fold excess of Cu(II) could be masked with EDTA. This method was successfully applied to the analysis of chromium(VI) in industrial effluents.