• Analytical Science and Technology
• /
• v.23 no.6
• /
• pp.572-578
• /
• 2010

The extraction/clean-up and concentrating of pharmaceuticals from surface water were performed by HLB (Hydrophilic-Lipophilic Balanced) cartridge. The method allows for the simultaneous determination of six pharmaceuticals by HPLC/ESI(+)-MS/MS. Recoveries of the pharmaceutical were between 71.1 to 92.6% (except fenbendazole) and the overall variability of the method was below 11.2% (RSD). The calibration curves for the pharmaceuticals from blank surface water showed good linearities (above $r^2$ = 0.99) in the concentration range of 0.007~1.2 ng/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 7.2~128.7 pg/mL and 23.8~429.1 pg/mL, respectively. The present analytical method can be useful for monitoring residual pharmaceuticals in surface water and other aquatic samples. High concentrations of iopromide and fenbendazole were detected in a few samples of surface water.

• Analytical Science and Technology
• /
• v.36 no.4
• /
• pp.143-151
• /
• 2023

Considering the greater role of α-amino acids in our daily lives, the enantiomer resolution of seven α-amino acids derivatized with fluorogenic reagent (4-fluoro-7-nitro-2,1,3-benzoxadiazole, NBD-F) by chiral HPLC on amylose or cellulose trisphenylcarbamate derived chiral stationary phases (CSPs) under simultaneous ultraviolet (UV) and fluorescence (FL) detection was performed. The degree of enantioseparation and resolution was affected by nature and selector backbones of the CSPs as well as the kind of amino acids. Baseline enantiomer separation and resolutions were observed for the enantiomers of all analytes as NBD derivatives especially on coated type amylose tris(3,5-dimethylphenylcarbamate) derived CSPs (Chiralpak AD-H and Lux Amylose-1). The other CSPs also showed good enantioselectivity except for the CSPs (Chiralpak IB, Chiralcel OD-H and Lux Cellulose-1) having cellulose tris(3,5-dimethylphenylcarbamate) as chiral selectors. The developed analytical chiral method was applied to determine the enantiomeric purity of seven commercially available L-α-amino acids and the impurities as D-forms were found to be in the range 0.08-0.87 %, respectively. The intra- and interday accuracy and precision assays showed high accuracy and precision of the developed analytical method. This chiral HPLC method for the enantiomer resolution of amino acids using fluorescent derivatization could be useful for the determination of enantiomeric purity of pharmaceuticals and biological study for amino acid type compounds among chiral drugs.

• Korean Journal of Environmental Agriculture
• /
• v.39 no.2
• /
• pp.130-137
• /
• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• Journal of Korean Society for Atmospheric Environment
• /
• v.7 no.2
• /
• pp.137-142
• /
• 1991

A method is developed for the simultaneous determination of dissolved iron, copper, and zinc in rainwater. The method involves 25-fold evaporative concentration, ion chromatographic separation and subsequent spectrophotometric detection after post-column reaction with 4-(2-pyridylazo) resorcinol. Analytical sensitivities, being defined by the slopes of calibration curves, are 0.93, 0.54, and 0.11 Abs/ $\mu$g/ml for iron, copper, zinc, respectively. Detection limits render around a few tenth of one ng/ml. Precisions evaluated by replicate analysis of real sample are better than 10% RSD. Due to the lack of certified standards for rainwater, the accuracy of the method could not be assessed directly. However, the results of this method agree well with those by inductively coupled plasma mass spectrometry. Analytical results for a suite of Seoul rainwaters are presented herein.

• Journal of Korean Society for Atmospheric Environment
• /
• v.18 no.6
• /
• pp.475-485
• /
• 2002

An analytical method was investigated for the meaiiurement of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) concentrations in air samples. Procedures required for column chromatographic clean up. silicagel (stage I) and gel permeation chromatography (stage II), were discussed. Identification and quantification of PCBs and OCPs were performed using a combination of gas chromatography/mass spectrometry/ selected ion monitoring. Recovery tests calculated from six samples are 68∼137% for PCBs and 58∼130% for OCPs except for endrin aldehyde. Instrumental detection limits determined for the PCBs and OCPs varied from 0.05 to 0.18 pg/m3 and from 0.71 to 16.82 pg/㎥, respectively. The method has been applied to the analysis of air samples collected at Ansung city, Kyonggi province, Korea. This method may serve as a screening protocol for the simultaneous determination of PCBs and OCPs in air.

• YAKHAK HOEJI
• /
• v.59 no.5
• /
• pp.222-229
• /
• 2015

Lithospermi radix, the dried roots of Litospermum erythrorhizon Sieboid et Zuccarini (Boraginaceae), has long been used to treat detoxification and inflammation. In this study, we isolated two main quinoid compounds, ${\beta}$-hydroxyisovalerylshikonin (1) and acetylshikonin (2) from L. erythrorhizon. As acetylshikonin is considered as a marker compound of L. erythrorhizon, a rapid analysis method for the simultaneous determination of quinoid compounds including 2 was also developed by HPLC (High Performance Liquid Chromatography) and validation of this analytical method. By the developed method, two quinoid marker compounds (${\beta}$-hydroxyisovalerylshikonin and acetylshikonin) were successfully quantified in 31 commercial samples which were collected from different regions. The contents were 0.20% (${\beta}$-hydroxyisovalerylshikonin) and 0.22% (acetylshikonin), respectively.

• Journal of Microbiology and Biotechnology
• /
• v.19 no.1
• /
• pp.83-92
• /
• 2009

Individual immunochromatographic assays (ICG) for ochratoxin A (OTA) and zearalenone (ZEA) were optimized and used in the development of a one-step simultaneous immunochromatographic assay (OS-ICG) for the rapid multianalysis of two mycotoxins in corn samples. The nitrocellulose membrane of the OS-ICG was treated with OTA-bovine serum albumin (BSA), ZEA-ovalbumin (OVA), and anti-mouse IgG in the OTA test, ZEA test, and control zones, respectively. Monoclonal antibody-gold conjugates (OTA3 MAb-gold and ZEA2C5 MAb-gold) were sprayed onto the conjugate pad. The visual detection limits were 2.5 and 5 ng/ml for OTA and ZEA, respectively, and the results were obtained within 15 min after starting the analysis. An efficient, simple, and rapid extraction method using 30% MeOH/PBS was established and validated by analyzing the corn samples spiked with OTA/ZEA mixtures (0/0, 5/10, 10/20, and $20/30\;{\mu}g/kg$). The cut-off values of the OS-ICG for the spiked corn were 5 and $10\;{\mu}g/kg$ for OTA and ZEA, respectively. Natural corn samples were analyzed by OS-ICG, direct competitive enzyme-linked immunosorbent assay (DC-ELISA), and HPLC. Results of the OS-ICG were in good agreement with those obtained by DC-ELISA and HPLC. The developed OS-ICG offers a rapid, easy-to-use, and portable analytical system and can be used as a convenient qualitative tool for the on-site simultaneous determination of OTA and ZEA in cereals, food, and agricultural products in one analytical cycle.

• Bulletin of the Korean Chemical Society
• /
• v.24 no.3
• /
• pp.285-290
• /
• 2003

An analytical method for the simultaneous determination of trace Ge, As and Se in biological samples by inductively coupled plasma/mass spectrometry has been investigated. The effects of added organic gas into the coolant argon gas on the analyte signal were studied to improve the detection limit, accuracy and precision. The addition of a small amount of methane (10 mL/min.) into the coolant gas channel improved the ionization of Ge, As and Se. The analytical sensitivity of the proposed Ar/CH₄system was superior by at least two-fold to that of the conventional Ar method. In the present method, the detection limits obtained for Ge, As and Se were 0.014, 0.012 and 0.064 ㎍/L, respectively. The analytical reliability of the proposed method was evaluated by analyzing the certified standard reference materials (SRM). Recoveries of 99.9% for Ge, 103% for As, 96.5% for Se were obtained for NIST SRM of freeze dried urine sample. The proposed method was also applied to the biological samples.

• Journal of the Korean Geosynthetics Society
• /
• v.9 no.4
• /
• pp.17-25
• /
• 2010

Evaluation of stability in traditional designing of reinforced soil structures is executed by examination of internal and external stability. Analysis of internal stability is for pull-out and ductile strength. Analysis of external stability is for settlement, overturning and sliding. To minimize inherent uncertainties of soil properties and analytical model, reliability analysis was developed recently. In this study, reliability analysis method considering simultaneous failure probability for various failure mode of internal and external stability is proposed. By applying uni-modal bounds, Stability of system reliability of reinforced soil structures is evaluated by integrating multi failure mode for various analytical model. Because of complex consideration for various failure shapes and modes, it is possible to secure advanced safety by using simultaneous failure probability. And evaluation of reinforced soil structure is executed by representative index, simultaneous failure probability, than previous method.

• Analytical Science and Technology
• /
• v.28 no.2
• /
• pp.112-116
• /
• 2015

Extraction of quaternary ammonium compounds (choline and betaine) from plant samples (spinach) using ion exchange resin (AG1, OH⁻ form) is a very simple and inexpensive approach. However, it is very hard to determine amounts of choline and betaine simultaneously using high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Unlike choline, betaine has low molar absorptivity in UV-visible (UV-Vis) region, which makes it difficult to carry out UV-Vis detection of betaine. The mixture of quaternary ammonium compounds (choline and betaine) was derivatized using 2-bromo acetophenone as a derivatizing agent. As a result, choline did not react with the derivatizing agent, whereas betaine formed a betaine derivative. This betaine derivative exhibited detectable UV absorption with baseline separation between choline and the betaine derivative. Thus, with this method, choline and betaine can be determined simultaneously by using the HPLCUV method through one-step derivatization, which is an easy, sensitive, and reliable method.