• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.242-256
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• 2012

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

• Bulletin of the Korean Chemical Society
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• v.22 no.4
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• pp.409-412
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• 2001

Poly(p-tert-butyltrimethoxymonopropyloxycalix[4]arene-methylsiloxane) (TBCX-MS) has been prepared and used as a stationary phase in isothermal capillary gas chromatographic separation of some positional isomers. Retention factors (k) and separatio n factors $(\alpha)$ for the isomers were measured and compared with those on poly(p-tert-butyl-dimethoxydipropyloxycalix[4]arene-tetramethyldisiloxane) (TBCX-TMDS), poly(dimethoxydipropyloxycalix[4]arenetetramethyl-disiloxane) (CX-TMDS). Most of the isomers investigated are well resolved on TBCX-MS. Retention of all the compounds decreases on the three phases in the order, TBCX-TMDS ${\geq}$ TBCX-MS > CX-TMDS. Similar retention values on TBCX-TMDS and TBCX-MS seem to indicate that retention property of the two phases is not significantly affected by the spatial position of the calixarene moiety.

• Mass Spectrometry Letters
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• v.14 no.3
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• pp.104-109
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• 2023

Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

• Archives of Pharmacal Research
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• v.23 no.6
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• pp.599-604
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• 2000

$\beta$-Sitosterol, campesterol and stigmasterol have been known to the phytosterols the most frequently found in plants. Metabolism of phytosterols was investigated using rat feces and liver microsomes. Feces were collected after phytosterols (a well characterized mixture of $\beta$-sitosterol 40%, campesterol 30% and dihydrobrasicasterol) were administered orally (0.5 ${g/kg$) to rats. Metabolites of phytosterols were identified using GC/MS. Three peaks were eluted at 12.47, 12.65, 12.87 min and had characteristic molecular ions m/z 428, 430, 432, respectively. Three fecal metabolites were identified as androstadienedione, androstenedione, and androstanedione. No metabolites could be detected in the rat liver microsomal reaction mixture. The results suggest that the metabolites of phytosterols in rat feces are formed by oxidation at 3- position, saturation at 5- and 6- position, and 17- side chain cleavage in the rat large intestine.

• Journal of Ginseng Research
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• v.21 no.3
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• pp.214-218
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• 1997

New simple methods for the Isolation of sesquiterpenes from Panax ginseng were developed. First, volatile compounds were isolated by simultaneous distillation and extraction (SDE) with 30% methanol and $\alpha$-hexane instead of water and ethyl ether/pentane (1:1). Secondly, head space volatiles in U-shaped tube at 7$0^{\circ}C$ were passed through C18 Sep-Pak by nitrogen gas streaming and the adsorbed volatiles were fluted by $\alpha$-hexane. TLC analysis showed that the volatile concentrates consisted mainly of terpenes when colored by vanillin-sulfuric and. GC/MS data revealed that approximately 30 sesquiterpenes of molecular weight 204 occupied 81.1% or more of the volatile concentrates isolated by those two newly developed methods. Among these, alloaromadendrene, germacrene B, isocaryophyllene, $\alpha$-neoclovene, ${\gamma}$-muurolene, $\beta$-panaslnsene, and $\alpha$-humulene were identified as being major sesqulterpenes by authentic samples or literatme search Key words : Panax ginseng, volatile compound, sesquiterpene, isolation, new method, GC/MS.

• Bulletin of the Korean Chemical Society
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• v.34 no.6
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• pp.1703-1707
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• 2013

A fast and simple sampling and sample preparation device, (NTD) has been developed and applied to sample and analyze volatile components from ground coffee beans. Coffee fragrances and other volatile organic compounds (VOCs) were sampled by the NTD and then analyzed by gas chromatograph-mass spectrometry (GC/MS). Divinylbenzene (DVB) particles (80/100 mesh size) were the sorbent bed of the NTD. More than 150 volatile components were first identified based on the database of the mass library and then finally 30 fragrances including caffeine were further confirmed by comparing experimental retention indices (i.e. Kovat index) with literature retention indices. Total sampling time was 10 minutes and no extra solvent extraction and/or reconstitution step need. Straight n-alkanes (C6-C20) were used as retention index probes for the calculation of experimental retention indices. In addition, this report suggests that an empty needle can be an alternative platform for analyzing polymers by pyrolysis-GC/MS.

• Bulletin of the Korean Chemical Society
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• v.26 no.12
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• pp.1996-2000
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• 2005

Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

• Korean Journal of Pharmacognosy
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• v.48 no.1
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• pp.46-50
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• 2017

This study was conducted to investigate the antioxidative activities and tyrosinase inhibition effects of fractions from the distilled water extract of Inonotus obliquus. Moreover, GC-MS based analysis with trimethylsilyl (TMS) derivatization was carried out for active compound in the extract of I. obliquus. In DPPH radical scavenging ability, $SC_{50}$ values of the ethyl acetate fraction was 0.393 mg/ml as a result of the most effective than other fractions. Meanwhile, aqueous fraction showed higher effect in tyrosinase inhibitoty activity. In GC-MS based analysis with TMS derivatization, 7 compounds including syringic acid, vanillic acid and protocatechuic acid were observed in ethyl acetate fraction, and oxalic acid is the main compound in aqueous fraction. As a result, it was confirmed that oxalic acid in aqueous fraction from the distilled water extract of I. obliquus was a compound showing tyrosinase inhibition effect.

• Journal of Sensor Science and Technology
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• v.23 no.5
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• pp.320-325
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• 2014

Volatile flavor compounds from milk were analyzed and identified by using the analysis methods of headspace solid phase microextraction gas chromatography/mass spectrometry (HSPME-GC/MS) and electronic nose (E-Nose) system. About 30 volatile compounds were identified by HSPME-GC/MS for the fresh and off-flavor milk samples. Also, the correlation between rancidity and ageing days of milk was obtained by the aid of principal component analysis algorithm. It shows that the E-Nose system can identify the various types of milk flavor. These results imply that the analysis method based on the E-nose system can apply to the quality control of milk flavor and the rancidity.

• Korean Journal of Pharmacognosy
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• v.23 no.1
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• pp.29-33
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• 1992

The essential oils of Lycopus lucidus have been studied. The essential oil obtained from the dried herba by steam distillation followed by fractionation by column chromatography was analysed by gas chromatography-mass spectrometry(GC-MS). The compounds identified by GC-MS were carvacrol, 2,5-dimethoxy-p-cymene, trans-caryophyllene, spathurenol and $trans-{\beta}-farnesene$. Two compounds, thymol and caryophyllene were isolated by silica gel column chromatography and analyzed by TLC, IR, Mass and NMR. And the weak diuretic effects of essential oil and water extract from the dried drugs were observed in rats.