• Archives of Pharmacal Research
• /
• 제26권9호
• /
• pp.697-705
• /
• 2003

The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

• 한국물환경학회지
• /
• 제32권6호
• /
• pp.670-699
• /
• 2016

In this study, 16 antibiotics were selected from among the top 30 veterinary antibiotics sold in South Korea in 2014, as well as from among the pharmaceuticals targeted by EPA method 1694, in order to review analytical methods for the detection of trace levels of antibiotics in environmental samples: surface water, soils, animal origin foods, and manures. LC-MS/MS was heavily used. In the chromatography for the detection of the selected antibiotics, the $C_{18}$ column was mostly used at the temperature of $30{\sim}40^{\circ}C$. Water and methanol/acetonitrile were commonly chosen as a nonpolar and a polar mobile phase, respectively. Gradient elution was applied to separate multiclass antibiotics. Volatile additives, such as formic acid, acetic acid, and ammonium acetate were mixed with the mobile phase to improve the ionization efficiency of analytes and the sensitivity in MS detection. Electrospray ionization (ESI) was widely used in the LC-MS/MS and positive ionization was preferred to determine the selected antibiotics. A protonated $[M+H]^+$ molecule was selected as a precursor ion, and its two transitions were analyzed, one for quantitative measurement and the other for confirmation. This study reviewed linearity of the calibration curve, recovery, repeatability, method detection limits (MDLs), and method quantification limits (MQLs) for each target compound used to validate the developed analytical methods.

• Bulletin of the Korean Chemical Society
• /
• 제30권1호
• /
• pp.61-66
• /
• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• 농약과학회지
• /
• 제5권1호
• /
• pp.19-23
• /
• 2001

수도용 제초제 butachlor의 작물잔류성을 조사할 목적으로 주산단지 및 광주, 대구, 부산지역의 시장에서 쌀, 보리, 마늘 양파, 딸기 등 106점의 시료를 채취하여 잔류량을 분석하였다. 제초제 butachlor가 등록되어 있는 작물의 수확물 중 쌀 27점과 보리 15점에서 butachlor가 검출되지 않았으며, 또한 벼 재배 후 이모작으로 재배되는 작물인 마늘21점, 양파 18점, 딸기 18점에서도 검출되지 않았다.

• Bulletin of the Korean Chemical Society
• /
• 제25권4호
• /
• pp.517-524
• /
• 2004

Two simple and sensitive spectrophotometric methods were developed for the determination of carbocisteine, penicillamine, ethionamide and thioctic acid in bulk and in their pharmaceutical preparations using alkaline potassium permanganate as an oxidizing agent. The first one involves determination of ethionamide and thioctic acid by spectrophotometric investigation of the oxidation reaction of the two drugs. The second method involves determination of carbocisteine and penicillamine by kinetic studies of the oxidation reaction of these two drugs at room temperature for a fixed time of 20 minutes. The absorbance of the colored manganate ions was measured at 610 nm in both methods. 1-10 ${\mu}$g/mL of ethionamide and thioctic acid could be etermined by the spectrophotometric method with detection limits of 0.11 and 0.089 ${\mu}$g/mL for the two drugs respectively. 2-10 ${\mu}$g/mL of carbocisteine and penicillamine could be determined by the kinetic method with detection limits of 0.14 and 0.21 ${\mu}$g/mL respectively. The two methods were successfully applied for the determination of these drugs in their dosage forms.

• Food Science and Biotechnology
• /
• 제18권4호
• /
• pp.978-984
• /
• 2009

An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.

• Bulletin of the Korean Chemical Society
• /
• 제29권2호
• /
• pp.352-356
• /
• 2008

An analytical method has been developed for measuring chlorostyrenes in fish tissue sample. Extraction of chlorostyrenes from fish tissue was carried out by ultrasonication using acetone/n-hexane (5:2, v/v) mixture. Most of the lipids in the extract were eliminated by freezing-lipid filtration, prior to solid-phase extraction (SPE) cleanup. During freezing-lipid filtration, about 90% of the lipids extracted from the fish samples were easily removed without any significant losses of chlorostyrenes. For purification, SPE using Florisil was used for the rapid and effective cleanup. Quantification was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery was above 80% in the spiked fish tissue sample at 10 and 100 ng/g levels, respectively. The detection limits for chlorostyrenes were ranged from 0.05 to 0.1 ng/g. This developed method is demonstrated to give efficient recoveries and LODs for detecting chlorostyrenes spiked into fish tissue with high lipid content.

• 한국환경과학회지
• /
• 제23권10호
• /
• pp.1693-1701
• /
• 2014

A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. $50/30{\mu}m$ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to $0.15{\mu}gL$ for VFAs and from 0.12 to $0.28{\mu}gL$ for indoles and the correlations observed ($R^2$) were 0.975~1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

• 품질경영학회지
• /
• 제38권3호
• /
• pp.354-362
• /
• 2010

This paper presents a non-linear control chart based on support vector machine regression (SVM-R) to improve the accuracy of fault detection of cyclic signals. The proposed algorithm consists of the following two steps. First, the center line of the control chart is constructed by using SVM-R. Second, we calculate control limits by variances that are estimated by perpendicular and normal line of the center line. For performance evaluation, we apply proposed algorithm to the industrial data of the chemical vapor deposition process which is one of the semiconductor processes. The proposed method has better fault detection performance than other existing method

• Archives of Pharmacal Research
• /
• 제19권6호
• /
• pp.562-565
• /
• 1996

The photoreactivity of twelve anthraquinone derivatives was examined to evaluate its usefulness as a photo-reagent for the analysis of ginsenosides using photoreduction fluorescence (PRF) detection method. Among the tested compounds, 2-tert-butylandthraquinone (TBAQ), 2-chloroanthraquinone (CAQ) and anthraquinone (AQ) showed good characteristics as photoreagents. The detection limits of ginsenoside $Rg_{1}$PRF-HPLC method using TBAQ, CAQ or AQ as a photo-reagent were found to be ca. 35 ng, 50 ng and 50 ng, respectively.