• Elastomers and Composites
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• v.39 no.4
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• pp.309-317
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• 2004

Synthesis of fullerene oxides [$C_{70}O_n$] ($n=1{\sim}3$ or n=1) in solid state by fullerene [$C_{70}$] and several oxidants such as 3-chloroperoxy benzoic acid, chromium(VI) oxide, benzoyl peroxide, and trichloroisocyanuric acid was taken place under microwave irradiation. The reactivity in solid state oi fullerene [$C_{70}$] with various oxidants under same microwave condition increased in the order of 3-chloroperoxy benzoic acid > chromium(VI) oxide > trichloroisocyanuric acid ${\simeq}benzoyl$ peroxide. The MALDI-TOF-MS, UV-visible spectra and HPLC analysis confirmed that the products of fullerene oxidation were [$C_{70}O_n$] ($n=1{\sim}3$ or n=1).

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

• Elastomers and Composites
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• v.40 no.1
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• pp.45-52
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• 2005

Synthesis or fullerene oxides[$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1) by fullerene[$C_{60}$] and several oxidants such as 3-chloroperoxy benzoic acid, benzoyl peroxide, trichloroisocyanuric acid, and chromium(VI) oxide took place under microwave irradiation. The reactivity in solid state of fullerene[$C_{60}$] with various oxidants under same microwave rendition increased in order or 3- chloroperoxy benzoic acid > benzoyl peroxide > trichloroisocyanuric acid $\simeq$chromium(VI) oxide. The MALDI-TOF-MS, UV-visible spectra and HPLC analysis confirmed that the products of fullerene oxidation were [$C_{60}(O)_n$] ($n=1{\sim}4$ or n=1).

• Elastomers and Composites
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• v.40 no.3
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• pp.174-180
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• 2005

Sonochemical synthesis of fullerene oxides $[C_{70}O_n](n=1{\sim}2)$ by fullerene$[C_{70}]$ and metal hexacarbonyl complexes $M(CO)_6$(M=Cr, Mo, W) took place under air atmosphere. The reactivity of fullerene$[C_{70}]$ and several metal hexacarbonyl complexes $M(CO)_6$(M=Cr, Mo, W) under same ultrasonic condition increased in the order of $Mo(CO)_6$ > $W(CO)_6$ > $Cr(CO)_6$. The MALDI-TOF-MS, UV-visible spectra, and HPLC analysis confirmed that the products of sonochemical reaction were $[C_{70}O_n](n=1{\sim}2)$.

• Corrosion Science and Technology
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• v.16 no.4
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• pp.161-166
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• 2017

The qualitative composition of active components of the corrosion inhibitor CGW-85567 was studied. It was found that С18:2 and С18:1 imidazolines and the corresponding imidazolin-amides are the major components. The HPLC/MS technique was developed for their determination in the water solutions of monoethylene glycol (MEG). Industrial application of the inhibitor showed that MEG solution retained high concentration of the inhibitor for a long time after ceasing its addition into pipelines. Low values of the partition coefficients (0.010-0.014) of imidazolines in the system "water solution of MEG (concentration of MEG 62-85% v/v) - gas condensate" have allowed to pass on from the technology of continuous pumping of the inhibitor into protected pipelines to the periodic dosing technology. Taking into account a long time of circulation in the system and high temperatures during MEG regeneration process possible degradation products of the inhibitor were studied. N, N-dimethyl-dodecanamine-1, and N, N-dimethyl-tetradecanamine-1 were identified as major degradation products of the corrosion inhibitor CGW-85567.

• Analytical Science and Technology
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• v.16 no.6
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• pp.488-498
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• 2003

By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

• Journal of Food Hygiene and Safety
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• v.31 no.2
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• pp.94-98
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• 2016

This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.

• Analytical Science and Technology
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• v.22 no.4
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• pp.326-335
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• 2009

A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

• Mass Spectrometry Letters
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• v.5 no.1
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• pp.24-29
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• 2014

An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.254-268
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• 2011

Fenoxycarb, pyriproxyfen and methoprene are juvenile hormone mimic insecticide. These insecticides have been widely used for mosquito, fly, scale insects, and Lepidoptera. The purpose of this study was to develop a simultaneous determination procedure of fenoxycarb, pyriproxyfen and methoprene residues in crops using HPLC-UVD/MS. These insecticide residues were extracted with acetone from representative samples of four raw products which comprised brown rice, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and then n-hexane/dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The analytes were quantitated by HPLC-UVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at 3 levels per crop. Mean recovery ratios were ranged from 80.0 to 104.3% in four representative agricultural commodities. The coefficients of variation were less than 4.8%. Quantitative limit of fenoxycarb, pyriproxyfen, and methoprene was 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of fenoxycarb, pyriproxyfen and methoprene in the agricultural commodities.