• Advances in concrete construction
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• v.3 no.4
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• pp.317-331
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• 2015

This paper presents the effect of different micro-silica (MS) contents of 5, 10 and 15 wt.% as partial replacement of cement on mechanical and durability properties of high volume fly ash - recycled aggregate concretes (HVFA-RAC) containing 50% class F fly ash (FA) and 35% recycled coarse aggregate (RCA) as partial replacement of cement and natural coarse aggregate (NCA), respectively. The measured mechanical and durability properties are compressive strength, indirect tensile strength, elastic modulus, drying shrinkage, water sorptivity and chloride permeability. The effects of different curing ages of 7, 28, 56 and 91 days on above properties are also considered in this study. The results show that the addition of MS up to 10% improved the early age (7 days) strength properties of HVFA-RAC, however, at later ages (e.g. 28-91 days) the above mechanical properties are improved for all MS contents. The 5% MS exhibited the best performance among all MS contents for all mechanical properties of HVFA-RAC. In the case of measured durability properties, mix results are obtained, where 10% and 5% MS exhibited the lowest sorptivity and drying shrinkage, respectively at all ages. However, in the case of chloride ion permeability a decreasing trend is observed with increase in MS contents and curing ages. Strong correlations of indirect tensile strength and modulus of elasticity with square root of compressive strength are also observed in HVFA-RAC. Nevertheless, it is established in this study that MS contributes to the sustainability of HVFA-RAC significantly by improving the mechanical and durability properties of concrete containing 50%less cement and 35% less natural coarse aggregates.

• Korean Journal of Environmental Agriculture
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• v.37 no.2
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• pp.117-124
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• 2018

BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

• Journal of Environmental Health Sciences
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• v.36 no.6
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• pp.510-517
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• 2010

Phthalates, such as di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) have been proved to be teratogenics and endocrine disruptors, metabolized rapidly and excreted in the urine. In this study, a simultaneous analytical method for 10 phthalate metabolites, MnBP, MiBP, MBzP, MCHP, MEHP, MEHHP, MEOHP, MnOP, MiNP and MiDP, in human urines, based on switching system with on-line pretreatment column using HPLC-MS/MS has been developed. This method was validated according to the guideline of bioanalytical method validation of National Institute of Toxicological Research. Limits of detection range between 0.2 and 0.9 ng/ml for 10 phthalate metabolites. The calibration curves showed linearity in the range 0.997~0.999, and the results of the intra- and inter-day validations were in the range from 0.4 to 14.7% RSD and from 0.3 to 9.4% RSD, respectively. Recoveries of phthalate metabolites varied from 87.0 to 116.1%. This analytical method showed high accuracy and stable precision for all metabolites, and seems to be suitable for biomonitoring of phthalates in human urine.

• Food Science of Animal Resources
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• v.41 no.1
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• pp.59-70
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• 2021

A method for simultaneous detection of fipronil (F) and its metabolites fipronil desulfinyl (FD), fipronil sulfide (FS), fipronil sulfone (FSO) in chicken eggs was applied and validated. It includes single-step, cheap, effective, rugged, safe-based method (SinChERS) for sample preparation and ultra high performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) for chemical analysis. Results suggested that formic acid enhanced the recovery of 4 target residues and 1% supplementation to acetonitrile gained higher recoveries than that of 5%. SinChERS integrated extraction and clean-up steps into one, with shorter time (1.5 h) to operate and higher recoveries (97%-100%) than HLB, Envi-Carb-NH2 and quik-easy-cheap-effective-rugged-safe method (QuEChERS), and it consumed the smallest volume of extracting solvent (10 mL) as QuEChERS. Quantitative analyses using external standard method suggested the linear ranges of 4 target compounds were 1-20 ㎍/L with R2 >0.9947. The limit of detection (S/N>3) and quantification (S/N>10) were 0.3 ㎍/kg and 1 ㎍/kg. Recoveries ranged from 89.0% to 104.4%, and the relative standard deviations (n=6) at 1, 10, and 20 ㎍/kg were lower than 6.03%. Thirty batches of domestic eggs (500 g each) were detected by the established SinChERS-based UHPLC-MS/MS and no target residues were detected in all samples. The method developed in this study is a rapid, sensitive, accurate and economic way for multi-residue analysis of fipronil and its metabolites in eggs.

• Asian-Australasian Journal of Animal Sciences
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• v.16 no.4
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• pp.534-540
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• 2003

This study was conducted to investigate the effect of supplementation of galacto-oligosaccharides (GOS) on methane emission, nutrient digestibility, energy utilization and blood metabolites by Holstein cows fed silages. In two sequential digestion and respiratory trials, two non-lactating Holstein cows were arranged to a balanced incomplete block design. Experimental diets consisted of two silage types; orchardgrass (Dactylis glomerata L.) based silage (OS), mixed silage (orchardgrass based silage and alfalfa (Medicago sativa L.) silage) (MS), while two GOS levels were without supplementation (0) and 2% of dry matter intake supplementation (2). Four combination diets were OS-0, OS-2, MS-0 and MS-2. Significant effects of silage types and GOS supplementation levels were not observed for DM and OM intake. Whereas the digestibility of OM, NDF and ADF was significantly (p<0.05) higher in cows fed OS with and without GOS compared cows fed MS diets. As percentage of GE intake, fecal energy loss for OS diets was significantly (p<0.05) declined than for MS diets. In contrast, cows fed MS diets had lower (p<0.05) urine energy loss as a proportion of GE intake compared to OS diets. Energy loss as CH4 and heat production was numerically increased when cows fed both OS and MS with GOS supplementation. Compared to OS, CH4 emission in cows fed MS was numerically decreased by 10.8 %. Methane conversion ratio (energy loss as CH4 per unit of GE intake) for OS-0, OS-2, MS-0 and MS-2 were 7.1, 7.2, 6.8 and 7.0, respectively. Plasma of glucose and urea-N concentration were significantly (p<0.05) elevated from 1 h to 6 h after feeding, otherwise total protein in plasma was declined (p<0.01) at 6 after feeding.

• Mass Spectrometry Letters
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• v.4 no.3
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• pp.47-50
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• 2013

An ultra-fast generic LC-MS/MS method was developed for high-throughput quantification of discovery pharmacokinetic (PK) samples and its reliability was verified. The method involves a simple protein precipitation for sample preparation and the analysis by ultra-fast generic LC-MS/MS with the ballistic gradient program and selected reaction monitoring (SRM) mode. Approximately 290 new chemical entities (NCEs) (over 10,000 samples) from 5 therapeutic programs were analyzed. The calibration curves showed good linearity in the concentration range of 1, 2 or 5 to 2000 ng/mL. No significant ion suppression was observed in the elution region of all the NCEs. When approximately 300 plasma samples were continuously analyzed, the peak area of internal standard was constant and reproducible. In the repeated analysis of samples, the plasma concentrations and the area under the curve (AUC) were consistent with the results from the first analysis. These results showed that the present ultra-fast generic LC-MS/MS method is reliable in terms of selectivity, sensitivity, and reproducibility and could be useful for high-throughput quantification and other bioanalysis in drug discovery.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.54 no.4
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• pp.404-410
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• 2021

Although, mouse bioassay for the monitoring of azaspiracids (AZAs) toxins in shellfish has been used previously, the reported method has low sensitivity and it is time-consuming. Recently, there is an interest in the quantitative analysis of AZAs using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The purpose of this study is to verify the simultaneous analysis of AZAs in shellfish and tunicate in Korea using LC-MS/MS. To validate the method, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and repeatability were determined. All standard compounds were analyzed within 7 min. The correlation coefficients (R²) of the standard solution was higher than 0.9995 (within the range of 0.8-10.0 ㎍/L). The LODs and LOQs of AZAs in shellfish were 0.08-0.16 ㎍/kg and 0.23-0.50 ㎍/kg, respectively. The accuracy and precision of the method for determining AZAs in shellfish were 87.1-93.0% and 1.23-4.91%, respectively. Consequently, the verified LC-MS/MS method is suitable to analyze AZAs in shellfish and tunicates in Korea.

• Analytical Science and Technology
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• v.10 no.4
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• pp.240-245
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• 1997

An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).

• Mass Spectrometry Letters
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• v.8 no.1
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• pp.14-17
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• 2017

The effect of cationization agent concentration on glycan detection via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was investigated using $Na^+$ ions in the form of NaCl as the cationization agent. NaCl solution concentrations ranging from 1 mM to 1 M were investigated. Glycans from ovalbumin were mixed with the cationization agent solution and the 2,5-dihydroxybenzoic acid (2,5-DHB) matrix solution in a volume ratio of 1:1:1. The resulting mixture was loaded onto the MALDI plate. Two MALDI-TOF MS instruments (Voyager DE-STR MALDI-TOF MS and Tinkerbell RT MALDI-TOF MS) were used for detection of glycans. The best detection, in terms of the number of identified glycans, the peak intensity, and the signal-to-noise (S/N) ratio, was obtained with NaCl concentrations of 0.01-0.1 M for both MALDI-TOF MS instruments.

• Mass Spectrometry Letters
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• v.6 no.2
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• pp.27-30
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• 2015

This article reviews the fundamentals of sample preparation used in matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). MALDI is a soft ionization method used to generate analyte ions in their intact forms, which are then detected in MS analysis. MALDI-MS boasts fast analysis times and easy-to-use operation. The disadvantages of MALDI-MS include the occurrence of matrix-associated peaks and inhomogeneous distribution of analyte within the matrix. To overcome the disadvantages of MALDI-MS, various efforts have been directed such as using different matrices, novel matrix systems, various additives, and different sample preparation methods. These various efforts will be discussed in detail. This article will benefit those who would like to obtain basic knowledge of MALDI sample preparation and those who would like to use MALDI-MS in their chemical analyses.