• Korean Journal of Food Science and Technology
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• v.26 no.6
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• pp.665-669
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• 1994

A rapid gas chromatographic (GC) profiling method was applied to dairy products (milk and cheeses) for the simultaneous analysis of volatile and nonvolatile organic acids. Cheese samples were first made into aqueous samples by dissolving in water. The aqueous samples were then extracted with organic solvents after the acidification and NaCI saturation. The organic layers (diethyl ether : hexane= 1 : 1) were extracted with $NaHCO_3$ saturated solution with subsequent solid-phase extraction of the aqueous phases using Chromosorb P column/diethyl ether followed by triethylamine treatment. The resulting triethylammonium salts of acids were directly converted into volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC, and GC-mass spectrometry. From milk and four cheese samples studied, 31 organic acids including 21 fatty acids and other hydroxy and dioic acids were tentatively identified. The amounts of the fatty acids were different among the kinds of cheese and thus the simplified retention index (RI) spectra of organic acids were useful for the visual pattern recognition of each sample, when the Direct Comparision method between cheese and a blind sample were attempted, it was quickly recognized to be a gouda cheese with the 999 ppt match quality value.

• Korean Journal of Environmental Agriculture
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• v.36 no.4
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• pp.269-278
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• 2017

BACKGROUND: The objective of this study was to evaluate screening method of residual multi pesticides in dead birds by Orbitrap high resolution mass spectrometry (HRMS) to identify the cause of death for birds. METHODS AND RESULTS: Extraction and clean-up method of residual pesticides in liver of dead birds was used QuEChERS (Quick Easy Cheap Effective Rugged and Safe) and method validations was conducted using liquid chromatography and gas chroamtography with triple-quadrupole mass spectrometer (LC/MS/MS and GC/MS/MS) Also, we were evaluated screening method for the determination of residual pesticides in liver of dead birds by LC and GC Orbitrap Mass Spectrometry. Results of method validations, Correlation coefficients of the matrix matched calibration curves were >0.978, and the method detection limits (MDLs) and limits of quantitation (LOQ) were 2.8~72.1 ng/g (18.4 ng/g on average) and 9.0~230 ng/g (58.5 ng/g on average). The accuracy ranged from 69.1%to 130% (103% on average), and the precision values were less than 14.8%(3.8%on average). The screening of residual pesticides in liver of dead birds by LC and GC Orbitrap HRMS was detected monocrotophos, carbofuran, carbosulfan, deltametrin, benfuracarb, carbofuran, phosphamidon, prochloraz in investigated samples. CONCLUSION: This results showed that accurate mass were extraction of residual pesticides in dead birds by Orbitrap HRMS. It suggested that this screening method is applicable to the residual pesticide analysis for the cause of death as a main tool.

• Environmental Analysis Health and Toxicology
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• v.18 no.1
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• pp.45-55
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• 2003

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid -phase extraction (SPE) with XAD -4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8％) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 ng/g in 2,4-dichlorophenol, 1.01 ∼ 1.17 ng/g in t-butylphenol,2.17 ∼ 5.84 ng/g in pentachlorophenol, 12.68 ∼ 14.88 ng/g in nonylphenol and 30.84 ∼ 153.72 ng/g in bisphenol A.

• Korean Journal of Food Science and Technology
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• v.43 no.1
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• pp.6-11
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• 2011

Vinyl chloride (VC) and vinylidene chloride (VDC), which may be present in poly(vinyl chloride) (PVC) and poly(vinylidene chloride) (PVDC) food packaging, were analyzed by using a headspace-gas chromatograph (GC)/mass spectrometer (MS) equipped with a PLOT Q column. 1-Chloropropane (1-CP) was used as an internal standard. The determinations of VC and VDC were carried out by monitoring the characteristic ions for each compound: m/z=61, 62, 64 and m/z=61, 96, 98, respectively. The method validated in this study can be suitable for the compliance test of EU regulation. Among 103 food packaging samples, VC and VDC were not detected, except in one PVDC food package. However, the detected level of VDC in the sample was below the EU regulatory specific limitation.

• Journal of Food Hygiene and Safety
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• v.33 no.5
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• pp.339-346
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• 2018

This study was conducted to monitor the current status of pesticide residues in a total of 297 agricultural products for raw juice from January 2017 to September 2017. Pesticide residues in samples were analyzed by multiresidue method for the determination of multiclass pesticide with an aim to detect 220 pesticides using GC/ECD, GC/NPD, TOF/MS, LC/PDA, LC/FLD, and LC/MS-MS. The analysis revealed the presence of nine pesticides in 14 samples. The detected pesticides were chlorpyrifos, cyflufenamid, chlorothalonil, pendimethalin, azoxystrobin, pyridalyl, imazalil, fludioxonil and procymidone. The kinds of detected crops were mandarin, carrot, apple, celery, chicory, orange and grape. Risk assessment evaluated human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake) of pesticides detected and the range of %ADI (the ratio of EDI to ADI) values was 0.0011~6.7087% and safety level.

• Proceedings of the Korean Environmental Health Society Conference
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• 2005.06a
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• pp.337-340
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• 2005

Ethylene oxide is a genotoxic carcinogen with widespread uses as industrial chemical intermediate and gaseous sterilant. 2-hydroxyethylated N-terminal valine in Hb is a good biomarker for biological monitoring of ethylene oxide exposure, because of its stability. We studied the determination method of (N-2-hydroxy-ethyl)valine in hemoglobin adduct by using GC/MS. PFPITC and TBMS were used as appropriate derivatives. Ethylene oxide formed Hb adducts as (N-2-hydroxy-ethyl)valine(HEV) in mouse with ethylene oxide inhalation exposure. Standard HEV can be synthesized with 2-amino-ethanol and 2-bromo-3-methylbutyric acid. GC/MS can measured them after derivatization with pentafluorophenylisothiocianate(PFPITC) and N-(tertiary butyl dimethylsiiyl)-N-methyl-trifluoroacetamide(TBDMS-TFA) by using Edman procedure. Concentrations of Hb adduct were proportionally increased with exposure levels. They were 230${\pm}$35(nmol g$^{-1}$ globin) and 410${\pm}$72(nmol $g^{-1}$ globin) at 200ppm and 400ppm ethylene oxide inhalation exposure, respectively.

• Korean Journal of Food Science and Technology
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• v.39 no.6
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• pp.715-720
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• 2007

The levels of butyltin compounds in poly(vinyl chloride) (PVC) food packaging using gas chromatography/mass spectrometry (GC/MS) were monitored. The analytical method, involving the ethylation with sodium tetraethylborate, was found to be selective and sensitive for mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT), validated by a $0.005\;{\mu}g/mL$ limit of detection (LOD), an $R^2>0.999$ for linearity, and >90% of recovery, respectively. Finally, none of the commercial food wraps and gaskets showed detectable levels of butyltin compounds.

• Journal of the Korean Society of Food Science and Nutrition
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• v.36 no.2
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• pp.201-208
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• 2007

Functional oils (FOs) were produced from commercial diacylglycerol oil and red yeast rice extracts from 80% ethanol for 1 hr in a shaking water bath at $35^{\circ}C$ and 175 rpm. FOs contained (A) 600, (B) 1200, (C) 1800, and (D) 2280 ppm of red yeast-rice extracts, respectively. The Hunter a value and b value were risen whereas L value was reduced along with the increase of extract concentration. Content of monacolin K and total phenolic compounds in FOs significantly increased according to the increase of extract concentration. The oxidation stability of FOs was observed by Rancimat at $98^{\circ}C$. Induction time decreased according to the increase of extract concentration. The major volatile compounds of FOs were compared using the electronic nose (EN) system and solid phase microextraction (SPME) method combined with gas chromatograph/mass spectrometry (GC/MS). EN was composed of 12 different metal oxide sensors. Sensitivities (Rgas/Rair) of sensors from EN were analyzed by principal component analysis (PCA), whose proportion was 99.66%. For qualitative or quantitative analysis of volatile compounds by SPME-GC/MS, the divinylbenzene/carboxene/polydimethyl-siloxane fiber and sampling temperature of $50^{\circ}C$ were applied.

• Journal of the Korean Society of Clothing and Textiles
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• v.29 no.12 s.148
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• pp.1608-1618
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• 2005

The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeration at $7^{\circ}C$ (LT), room temperature (RT), oven treatment at $100^{\circ}C$ (OV), and $H_2O_2/UV(PER)$ method. Degradation times for each thermal system were 6 hour, 24 hour, 48 hour, 1 week, 2 week, 4 week. Alizarin was detected from the control and degraded samples of both alizarin dyed and madder dyed fabrics. Benzoic acid, 2, 4-di-tert-butylphenol, phthalic anhydride were detected as the degradation products for both alizarin dyed and madder dyed fabrics. The result suggest that these products can be used as the fingerprints of GC-MS analysis for the identification of madder dye in archaeological textiles. Both alizarin dyed and madder dyed samples became less red and less yellow after degradation. In the PER degradation system madder dyed sample showed the greatest color difference even after 1 week of degradation treatment. Further research is necessary for investigating the color change in the exhumed textiles, which is caused by the dual action of dye fading and the staining of organic matters in the soil.

• Journal of The Korean Society of Inherited Metabolic disease
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• v.15 no.2
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• pp.65-71
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• 2015

Since the secretion of specific chiral isomers in urine (or plasma) is very crucial to diagnose some inborn metabolic disorders, clinical application of dual column achiral differential method has been performed for the absolute configuration of chiral compounds. Extracted from the acidified urine with diethyl ether, carboxylic functional group of organic acid (stereoisomers of the volatile) was derivatized with (-)-menthylation or (S)-(+)-3-methyl-2-butylation and followed by O-trifluoroacylation. Each of the enantiomers was accurately separated from the library matched double column (achiral) with a retention index (I). In various inborn metabolic disease urines, absolute chirality was identified correctly in the urine (10 patients) with inborn metabolic disease (including secretion of D, L- lactic acid, D, L-3-hydroxybutyric acid, and D, L-2-hydroxyglutaric acid). In this study, we identified and isolated the volatile diastereomer as a useful diagnostic marker, this successful application to urine specimens may be useful for diagnostic classification of inherited metabolic disorders.