• Journal of The Korean Society of Inherited Metabolic disease
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• v.17 no.2
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• pp.39-47
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• 2017

Purpose: A sensitive gas chromatography mass spectrometry (GC-MS) method was developed for screening of fatty acid oxidation disorders. Methods: The assay utilized a simple protein precipitation with sulfosalicylic acid followed by tert-butyl dimethylsilyl (TBDMS) derivatization of hydroxyl functional group by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA). Results: Calibration curves of spiked pooled plasma showed a linear relationship in the range of 0.01 ng -2 mg with correlation coefficient value greater than 0.98. Limits of detection (LOD) and limits of quantification (LOQ) were found in the range of 0.9-8.8 ng and 9-88 ng, respectively. Conclusion: The new developed method might be useful for a rapid, sensitive screening of inherited fatty acid oxidation disorders. In addition, the method expected to be one of the alternative method for screening newborns of metabolic disorders in the laboratories where expensive MS/MS is unavailable.

• Journal of Environmental Health Sciences
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• v.32 no.1 s.88
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• pp.67-70
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• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

• Mass Spectrometry Letters
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• v.7 no.1
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• pp.26-29
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• 2016

Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r² value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

• Bulletin of the Korean Chemical Society
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• v.32 no.4
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• pp.1221-1227
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• 2011

Ethyl pyruvate (EP) is known as a scavenger of reactive oxygen species (ROS) in the body through its role in the donation of diketone groups to metals to form an EP-metal complex. In order to develop a method for the quantification of EP in biological media, a sensitive and specific, high-performance liquid chromatographyelectrospray ionization-mass spectrometry (HPLC-ESI/MS) method is used to determine the EP-alkali metal ion binding species. The analyte was separated on a ZORBOX SB-C8 ($3.5{\mu}m$, $30mm{\times}2.1mm$ I.D.) column and analyzed in selected ion monitoring (SIM) mode with a positive ESI interface using the m/z 255 $[2M + Na]^+$ ion. The method was validated over the concentration range of $0.5-60.0\;{\mu}g$/mL under 1/9 (v/v) of acetonitrile/methanol solvent system with flow rate 0.05 mL/min. The limit of quantification (LOQ) was $0.5{\mu}g$/mL.

• Toxicological Research
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• v.31 no.3
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• pp.265-271
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• 2015

This study was carried out to investigate contents of 8 polycyclic aromatic hydrocarbons (PAHs) from frequently consumed seafood and dairy products and to evaluate their chemical analysis methods. Samples were collected from markets of 9 cities in Korea chosen as the population reference and evaluated. The methodology involved saponification, extraction with n-hexane, clean-up on Sep-Pak silica cartridges and gas chromatograph-mass spectrometry analysis. Validation proceeded on 2 matrices. Recoveries for 8 PAHs ranged from 86.87 to 103.57%. The limit of detection (LOD) 8 PAHs was $0.04{\sim}0.20{\mu}g/kg$, and limit of quantification (LOQ) of 8 PAHs was $0.12{\sim}0.60{\mu}g/kg$. The mean concentration of benzo[a]pyrene (BaP) was $0.34{\mu}g/kg$ from seafood and $0.34{\mu}g/kg$ from dairy products. The total PAHs concentration was $1.06{\mu}g/kg$ in seafood and $1.52{\mu}g/kg$ in dairy products.

• Environmental Engineering Research
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• v.13 no.4
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• pp.216-223
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• 2008

An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

• Bulletin of the Korean Chemical Society
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• v.35 no.3
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• pp.765-769
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• 2014

An analytical methodology was developed for qualitative and quantitative impurity profiling of the coloring agent Sudan III by high-performance liquid chromatography (HPLC)-diode array detection (DAD). The impurities in commercial Sudan III were characterized by comparison of their retention times and UV spectra with those of authentic standards. Four impurities regulated by International Committees in Sudan III were quantified by HPLC-selective UV detection. The impurities in Sudan dye were successfully separated on a reversed phase C18-column within 25 min and sensitively detected by UV spectrometry at two selective wavelengths. Method validation was conducted to determine linearity, precision, accuracy, and limit of quantification (LOQ). The linear dynamic range extended from 0.002 to 4.0%, with a correlation coefficient (R2) greater than 0.995. The LOQs of the impurities ranged from 8.04 to $54.29{\mu}g/mg$. Based on the established method, the levels of regulated impurities in five commercial Sudan III dyes were determined.

• Korean Journal of Pharmacognosy
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• v.40 no.3
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• pp.224-228
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• 2009

For the quality control of traditional herbal medicine, Galgeun tang, simultaneous determination of glycyrrhizin, paeoniflorin, puerarin, 6-gingerol was established by using a high performance liquid chromatographic (HPLC) method with diode array detector. To separate five four constituents, DIONEX $C_{18}$ column ($5{\mu}m$, $120{\AA}$, $4.6\;mm{\times}150\;mm$) was used with gradient elution system of water and methanol. Validation of the chromatography method was evaluated by linearity, recovery, and precision test. Calibration curve of standard components showed excellent linearity ($R^2$>0.9906). Limits of detection (LOD) and limits of quantification (LOQ) varied from 0.15 to $0.52{\mu}g$/ml and 0.27 to $0.80{\mu}mg$/ml, respectively. The relative standard deviations (RSDs) of data of the intra-day and inter-day experiments were less than 2.88% and 1.21%, respectively. The results of recovery test were ranged from 96.71 to 106.29% with RSD values 0.01-0.80%.

• Bulletin of the Korean Chemical Society
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• v.28 no.3
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• pp.369-372
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• 2007

A fast and simple high-performance liquid chromatography (HPLC) method for the simultaneous determination of four pesticides having fungicide properties has been proposed for Panax ginseng, C. A. Meyer grown for 4, 5, or 6 years. Analytical separation was performed on C18 columns using ultraviolet detector under gradient conditions. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The HPLC response for all pesticides was linear, with determination coefficients > 0.9986. The average rate of recovery for pesticides spiked with 2 fortification levels was > 72% with relative standard deviations < 9%. The limits of quantification (LOQ) ranged from 0.03 to 0.16 ppm. These LOQs were lower than the respective maximum residue limits (MRL) established by the Korean Food and Drug Administration (KFDA), except for cyazofamid. The proposed method was used to determine pesticide residue levels in samples of ginseng obtained from Jeonnam Province (Republic of Korea). None of the pesticides were found in ginseng samples grown for 4, 5, or 6 years.

• YAKHAK HOEJI
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• v.56 no.3
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• pp.145-151
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• 2012

To develop fundamental data of herbal materials with heat treatment, we studied analytical and extraction methods of benzopyrene in black ginseng and validated by HPLC analysis. Benzopyrene was successfully separated in mobile phase of acetonitrile:water (80 : 20) and detection of excitation 294 nm, emission 404 nm. The calibration curve of benzopyrene was linear over the concentration range of 1.17~37.50 ng/ml with correlation coefficient of above 0.999. The limit of detection (LOD) and quantitation (LOQ) of benzopyrene was 0.25 and 0.75 ng/ml, respectively. Hexane extraction method was used as a new extraction method for benzopyren and the efficient of extraction was over 95%. In conclusion, analytical method and extraction method were suitable for the determination of benzopyrene in the black ginseng and could be applied to fundamental study and guideline of herbal materials with heat treatment.