• Analytical Science and Technology
• /
• v.20 no.5
• /
• pp.424-433
• /
• 2007

An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

• Microbiology and Biotechnology Letters
• /
• v.40 no.1
• /
• pp.57-65
• /
• 2012

Antifungal compounds from Bacillus polyfermenticus CJ6 were purified using SPE, preparative HPLC, and reverse phase-HPLC. Antifungal compounds from B. polyfermenticus CJ6 were separated into three fractions (8, B, C) using preparative HPLC. LC/MS analysis of antifungal peaks suggested that B. polyfermenticus CJ6 produces lipopeptides; two kinds of iturin A ($C_{14}$, $C_{15}$), three kinds of surfactins ($C_{13}$, $C_{14}$, $C_{15}$), four kinds of fengycin A ($C_{14}$, $C_{15}$, $C_{16}$, $C_{17}$) and two kinds fengycin B ($C_{16}$, $C_{17}$). The antifungal activity of fraction 8, which was presumed as inturin A, was found to be stable after the pH, heat or proteolytic enzyme treatment, but it was unstable at 50-$70^{\circ}C$ for 24 hr. The antifungal activity of fraction B, which presumed as surfactins and fengycin A, was found to be stable after the heat treatment, but it was unstable in the pH 3.0 and after the protease (type I) or ${\alpha}$-chymotrypsin treatment. The antifungal activity of fraction C, which was presumed as fengycin A and B, was found to be stable in the pH 3.0-9.0 range and the heat treatment, but it was unstable with the treatment of protease (type I). The amino acid composition of the purified peaks 8-1 and 8-2 were Asx, Tyr, Gln, Pro, and Ser in a molar ratio of 3:1:1:1:1, which showed the same amino acid composition as iturin. From these results, we confirmed that antifungal compounds from B. polyfermenticus CJ6 most likely belonged to iturin A as well as surfactins and fengycins. As lipopeptides are known to act in a synergistic manner, the antifungal compounds from B. polyfermenticus CJ6 might have potential uses in biotechnology and biopharmaceutical applications.

• The Korean Journal of Pesticide Science
• /
• v.17 no.2
• /
• pp.107-116
• /
• 2013

Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.

• Analytical Science and Technology
• /
• v.24 no.3
• /
• pp.225-230
• /
• 2011

Anatoxin-a is a cyanobacterial neurotoxin with a high toxicity produced by Anabaena, Aphanizomenon and Oscillatoria. Water bloom, formed by Anabaena has been occurring frequently in Lake Yeongchun. It is need to develop a sensitive method for determination of anatoxin-a to control potential hazard in raw water resources. In this study, we developed a highly sensitive analytical method of anatoxin-a using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. Anatoxin-a was converted into a highly fluorescent derivative using 4-fuoro-7-nitro-2,1,3-benzoxadiazole (NBF-F). The method was evaluated in terms of linearity of calibration curve, recovery and repeatability, and the adequate values were obtained. The method detection limit was $0.034\;{\mu}g/g$ and $0.022\;{\mu}g/L$ for algal and water samples, respectively. The concentrations of anatoxin-a were measured in algal and water samples from Lake Andong, Yeongchun and Daechung and ranged from $0.135\;{\mu}g/g$ to $10.979\;{\mu}g/g$ in algal samples and not detected in water samples.

• Food Science and Biotechnology
• /
• v.14 no.5
• /
• pp.586-592
• /
• 2005

This study was performed to investigate the antioxidant effects of Korean soybean paste extracts (SPE) on 2,2-azobis (2-amidinopropane) dihydrochloride (AAPH)-induced liver damage in rats. Thirty healthy Sprague Dawley rats were selected and divided into 5 groups. Isoflavone contents were measured using HPLC technique. The antioxidant activity was measured in the plasma and liver of the rats with the following results. Levels of isoflavone in fermented soy paste, red pepper paste and soy sauce were 28.9, 30.3 and $3.4\;{\mu}g/g$ for daidzein and 244.3, 187.7 and $6.1\;{\mu}g/g$ for genistein, respectively. The activities of glutamate oxaloacetic transaminase (GOT) and glutamate pyruvate transaminase (GPT) were significantly higher in the AAPH-treated group in the SPE-AAPH group (p<0.05). The thiobarbituric acid reactive substance (TBARS) production was significantly increased in the AAPH-treated liver tissue (P<0.05). Glutathione peroxidase (GPx), glutathione reductase (GR) and catalase in the liver were significantly (p<0.05) decreased by AAPH administration. The glutathione (GSH) concentration was higher in the SPE-treated (Ed- confirm) group than in the control and other groups (p<0.05). These results suggest that SPE led to increased anti oxidative activities against AAPH-induced peroxyl radical.

• Journal of Electrochemical Science and Technology
• /
• v.14 no.1
• /
• pp.1-14
• /
• 2023

The overuse of pesticides in agricultural sectors exposes people to food contamination. Pesticides are toxic to humans and can have both acute and chronic health effects. To protect food consumers from the adverse effects of pesticides, a rapid monitoring system of the residues is in dire need. Molecularly imprinted polymer (MIP) on a screen-printed electrode (SPE) is a leading and promising electrochemical sensing approach for the detection of several residues including pesticides. Despite the huge development in analytical instrumentation developed for contaminant detection in recent years such as HPLC and GC/MS, these conventional techniques are time-consuming and labor-intensive. Additionally, the imprinted SPE detection system offers a simple portable setup where all electrodes are integrated into a single strip, and a more affordable approach compared to MIP attached to traditional rod electrodes. Recently, numerous reviews have been published on the production and sensing applications of MIPs however, the research field lacks reviews on the use of MIPs on electrochemical sensors utilizing the SPE technology. This paper presents a distinguished overview of the MIP technique used on bare and modified SPEs for the detection of pesticides from four recent publications which are malathion, chlorpyrifos, paraoxon and cyhexatin. Different molecular imprint routes were used to prepare these biomimetic sensors including solution polymerization, thermal polymerization, and electropolymerization. The unique characteristics of each MIP-modified SPE are discussed and the comparison among the findings of the papers is critically reviewed.

• Journal of Radiopharmaceuticals and Molecular Probes
• /
• v.2 no.2
• /
• pp.103-107
• /
• 2016

Solid phase extraction (SPE) purification method is the efficient and well-known tool for automated [$^{11}C$]acetate synthesis. A fully automated homemade module adopting the SPE method and 'pinch' valves was developed very economically with a universal interface board, a relay card and an open source programmable logic controller. The radiochemical yield of the optimized [$^{11}C$]acetate synthesis by this system was $58.8{\pm}2.1%$ (n=10, decay-corrected) from $15.5{\pm}0.19GBq$ of $[^{11}C]CO_2$ as starting activity, and total synthetic time was 15 minutes. HPLC analysis showed its high radiochemical purity as $97.4{\pm}1.1%$ without possible by-products.

• Asian-Australasian Journal of Animal Sciences
• /
• v.14 no.10
• /
• pp.1465-1469
• /
• 2001

A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.48 no.6
• /
• pp.429-433
• /
• 2003

trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

• Journal of Food Hygiene and Safety
• /
• v.31 no.3
• /
• pp.186-193
• /
• 2016

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.