• Analytical Science and Technology
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• v.12 no.5
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• pp.1065-1077
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• 1999

• Analytical Science and Technology
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• v.6 no.1
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• pp.1003-1021
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• 1993

• Analytical Science and Technology
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• v.32 no.3
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• pp.88-95
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• 2019

This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

• Analytical Science and Technology
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• v.12 no.6
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• pp.521-527
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• 1999

In this study, capillary columns for ion chromatography were developed to analyze trace amount of ions in samples. When small I.D. capillary columns are used in ion chromatography, the typical flow rate of the mobile phase is $5{\sim}15{\mu}L/min$ and the typical column length is 50~150 mm. The capillary columns were made using RSL-300 fused silica capillary(I.D.: 0.53 mm, O.D.: 0.67 mm) and AG14 column resin(support : polystyrene-divinylbenzene, functional group : alkyl quaternary ammonium). The new conductivity cell and suppressor were also developed and made for capillary column ion chromatography. When several anions (fluoride, nitrite, nitrate, chlorate) were analyzed using these capillary columns, reproducible and good chromatograms were obtained.

• Analytical Science and Technology
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• v.10 no.5
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• pp.325-331
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• 1997

Among various CE separation methods, micellar electrokinetic capillary chromatography(MECC) method using sodium dodecylsulfate(SDS) provides rapid and accurate separation of organic explosive constituents with easy. The running buffer was composed with 2.5 mM borate and 25mM SDS(pH 8.5). Addition of 1M urea and 10% organic modifiers (acetonitrile, methanol and ethanol) improves the resolution of adjacent explosive constituents. When 15 explosive constituents were developed in MECC, most constituents were separated successively while RDX/TNB and DNN/DEP were not, and detection limits of separated compounds are in range of 1 to 4 ppm.

• Analytical Science and Technology
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• v.15 no.3
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• pp.190-195
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• 2002

We analysed mutation of ${\beta}_2$-adrenergic receptor gene that controls bronchial asthma by denaturing high performance liquid chromatography (DHPLC) according to ion-pair reversed-phase high performance liquid chromatography (IP-RP-HPLC). We extracted genomic DNA from 50 asthma patients, amplified DNA using PCR, and analysed PCR product by DHPLC. As a result, we obtained that mutation frequency was 15 (30%) among 50 cases. Consequently DHPLC mutation detection was confirmed that the result of direct sequencing was coincide exactly.

• Korean Journal of Food Science and Technology
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• v.39 no.5
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• pp.488-493
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• 2007

A survey for total aflatoxins (aflatoxins $B_1$, $B_2$, $G_1$, and $G_2$) was conducted on 245 cereals and processed cereal products, and 148 nuts and processed nut products in Korea, for a total of 393 commercialized ed samples. The total aflatoxins were quantified by the immunoaffinity column clean-up method with high performance liquid chromatography (HPLC) - fluorescence detection (FLD), and were confirmed by liquid chromatography tandem mass spectrometry (LC-MS/MS). Total aflatoxins(AFs) were detected in 37 samples (9.4% incidence), including 2 millet samples, 1 mixed cereal (sunsik), 1 powdered malt sample, 2 processed cereal products, 6 peanut samples, 22 peanut butter samples, and 1 sample each of almonds, adlay tea, and a processed nut product. The contamination levels were $0.04-2.65{\mu}g/kg$ for aflatoxin $B_1$, and $0.04-5.51{\mu}g/kg$ for total aflatoxins. Finally, LC-MS/MS analysis of the contaminated samples was conducted to confirm the detected aflatoxins, and all 37 samples showing aflatoxins by HPLC-FLD were confirmed by LC-MS/MS.

• Korean Journal of Food Science and Technology
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• v.40 no.3
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• pp.354-359
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• 2008

A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

• Analytical Science and Technology
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• v.10 no.5
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• pp.350-356
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• 1997

Supercritical Fluid Chromatography(SFC) has been developed as an analytical technique for the compounds that is difficult to analyze by conventional chromatography. Since supercritical fluid $CO_2$ is difficult to elute solutes with high polarity, modified supercritical $CO_2$, was used as a mobile phase. In conventional method, silica column which is saturated with modifier was used. However, with this method, we can not control the quantity of modifier. In this paper, we developed a new method which can control quantity of modifier mixed in supercritical fluid $CO_2$. The quantity of $H_2O$ mixed was measured with amperometric microsensor which was made by perflurosulfonate ionomer(PFSI) film. we have also obtained a good supercritical fluid chromatogram of PAH mixture by use of a modifier composition programming method.

• Analytical Science and Technology
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• v.26 no.6
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• pp.357-363
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• 2013

Selenium-containing proteins were separated from selenium-enriched yeast (SEY) using Trizol$^{(R)}$ reagent followed by anion exchange (AE) chromatography. This method is simpler and less time consuming than electrophoresis. Five selenium containing proteins were identified by on-line AE HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry). Each protein was enzymatically hydrolyzed to seleno-amino acids and separated with RP (reverse phase) HPLC for the identification of selenoproteins.