A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.
Flowable composite resin has lower filler content, increased flow, and lower modules of elasticity. It is suggested that flowable composite resin can be bonded to the tooth structure intimately and absorb or dissipate the stress. Therefore, it may be advantageous to use flowable composite resin for the base material of class II restoration and for the class V restoraton. The purpose of this study was to evaluate the microleakage and shear bond strength of four flowable composite resins (Aeliteflo, Flow-It, Revolution, Ultraseal XT Plus) compared to Z100 using Scotchbond Multi Purpose dentin bonding system. To evaluate the microleakage, notch-shaped class V cavities were prepared on buccal and lingual surfaces of 80 extracted human premolars and molars on cementum margin. The teeth were randomly divided into non-thermocycling group (group 1) and thermocycling group (group 2) of 40 teeth each. The experimental teeth of each group were randomly divided onto five subgroups of eight samples (sixteen surfaces). The Scotchbond Multi-Purpose and composite resin were applied for each group following the manufacturer's instructions. the teeth of group 2 were thermocycled five hundred times between 5$^{\circ}C$ and 55$^{\circ}C$. The teeth of group 2 were placed in 2% methylene blue dye for 24 hours, then rinsed with tab water. The specimens were embedded in clear resin, and sectioned longitudinally with a diamond saw. The dye penetration on each of the specimen were observed with a stereomicioscope at $\times$20 magnification. To evaluate the shear bond strength, 60 teeth were divided into five groups of twelve teeth each. The experimental teeth were ground horizontally below the dentinoenamel junction, so that no enamel remained. After applying Scotchbond Multi-Purpose on the dentin surface, composite resin was applied in the shape of cylinder. The cylinder was 4mm in diameter and 2mm in thickness. Shear bond strength was measured using Instron with a cross-head speed of 0.5mm/min. After shear bond strength measurement, mode of failure was evaluated with a stereomicroscope at $\times$30 magnification. All data were statistically analyzed by One Way ANOVA and Student-Newman-Keuls method. The correlation between microleakage and shear bond strength was analyzed by linear regression. The results of this study were as follows ; 1. In non-thermocycling group, the leakage value of Z100 was significantly lower than those of flowable composite resins at the enamel and dentin margin, margin, except that Revolution showed the lower leakage value than that of Z100 at the dentin margin (p<0.05). 2. In thermocycling group, the leakage values of Z100 and Ultraseal XT Plus were lower than those of other subgroup at the enamel and dentin margin, except that Flow-It showed the lower leakage value than that of Ultraseal XT Plus at the dentin margin (p<0.05). 3. The leakage value of Z100 and Ultraseal XT Plus in thermocycling group were not higher than that in non-thermocycling group at the enamel margin. The leakage value of Z100 in thermocycling group was not higher than that in non-thermocycling group at the dentin margin (p<0.05). 4. As for the shear bond strength measurement, there were no statistically significant differences among groups (p<0.05). The shear bond strengths given in descending order were as follows: Z100(16.81$\pm$2.98 MPa), Flow-It(14.8$\pm$4.43 MPa), Aeliteflo(14.34$\pm$3.69 MPa), Revolution(13.46$\pm$4.23 MPa), Ultraseal XT Plus(12.83$\pm$3.16 MPa). 5. Failure modes of all specimens were adhesive failures. 6. There was no correlation between microleakage and shear bond strength.
Kim, Yun-Ju;Jin, Myoung-Uk;Kim, Sung-Kyo;Kwon, Tae-Yub;Kim, Young-Kyung
Restorative Dentistry and Endodontics
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v.33
no.3
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pp.169-176
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2008
The purpose of this study was to evaluate the effect of thickness, filling methods and curing methods on the polymerization of dual cured core materials by means of microhardness test. Two dual cured core materials, MultiCore Flow (Ivoclar Vivadent AG, Schaan, Liechtenstein) and Bis-Core (Bisco Inc., Schaumburg, IL, USA) were used in this study. 2 mm (bulky filled), 4 mm (bulky filled), 6 mm (bulky and incrementally filled) and 8 mm (bulky and incrementally filled)-thickness specimens were prepared with light cure or self cure mode. After storage at $37{\circ}C$ for 24 hours, the Knoop hardness values (KHN) of top and bottom surfaces were measured and the microhardness ratio of top and bottom surfaces was calculated. The data were analyzed using one-way ANOVA and Scheffe multiple comparison test, with ${\alpha}$= 0.05. The effect of thickness on the polymerization of dual cured composites showed material specific results. In 2, 4 and 6 mm groups, the KHN of two materials were not affected by thickness. However, in 8 mm group of MultiCore Flow, the KHN of the bottom surface was lower than those of other groups (p < 0.05). The effect of filling methods on the polymerization of dual cured composites was different by their thickness or materials. In 6 mm thickness, there was no significant difference between bulk and incremental filling groups. In 8 mm thickness, Bis-Core showed no significant difference between groups. However, in MultiCore Flow, the microhardness ratio of bulk filling group was lower than that of incremental filling group (p < 0.05). The effect of curing methods on the polymerization of dual cured composites showed material specific results. In Bis-Core, the KHN of dual cured group were higher than those of self cured group at both surfaces (p < 0.05). However, in MultiCore Flow, the results were not similar at both surfaces. At the top surface, dual cured group showed higher KHN than that of self cured group (p < 0.05). However, in the bottom surface, dual cured group showed lower value than that of self cured group (p < 0.05).
The objectives of this study was to evaluate the effect of thermocycling on the ${\mu}TBS$ (microtensile bond strength) to dentin with four different adhesive systems to examine the bonding durability. Freshly extracted $3^{rd}$ molar teeth were exposed occlusal dentin surfaces, and randomly distributed into 8 adhesive groups 3-steps total-etching (Scotchbond Multi-Purpose Plus; SM, All Bond-2; AB), 2-steps total-etching (Single Bond; SB, One Step plus; OS), 2-steps self-etching (Clearfil SE Bond; SE, AdheSE AD) and single-step self-etching systems (Promp L-Pop; PL, Xeno III; XE) Each adhesive system in 8 adhesives groups was applied on prepared dentin surface as an instruction and resin composite (Z250) was placed incrementally and light-cured. The bonded specimens were sectioned with low-speed diamond saw to obtain $1\times1mm$ sticks after 24 hours of storage at $37^{\circ}C$ distilled water and proceeded thermocycling at the pre-determined cycles of 0, 1,000 and 2,000. The ${\mu}TBS$ test was carried out with EZ-tester at 1mm/min. The results of bond strength test were statistically analyzed using one-way ANOVA/ Duncan's test at the a < 0.05 confidence level. Also, the fracture mode of debonded surface and the interface were examined under SEM. The results of this study were as follows ; 1. 3-step total etching adhesives showed stable, but bond strength of 2-step adhesives were decreased as thermocycling stress. 2. SE showed the highest bond strength, but single step adhesives (PL, XE) had the lowest value both before and after thermocycling. 3 Most of adhesives showed adhesive failure. The total-etching systems were prone to adhesive failure and the single-step systems were mixed failure after thermocycling. Within limited results of this study, the bond strength of adhesive system was material specific and the bonding durability was affected by the bonding step/ procedure of adhesive Simplified bonding procedures do not necessarily imply improved bonding performance.
Proceedings of the Korean Institute of Surface Engineering Conference
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2000.11a
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pp.3-4
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2000
Many researchers are interested in the synthesis and characterization of carbon nitride and diamond-like carbon (DLq because they show excellent mechanical properties such as low friction and high wear resistance and excellent electrical properties such as controllable electical resistivity and good field electron emission. We have deposited amorphous carbon nitride (a-C:N) thin films and DLC thin films by shielded arc ion plating (SAIP) and evaluated the structural and tribological properties. The application of appropriate negative bias on substrates is effective to increase the film hardness and wear resistance. This paper reports on the deposition and tribological OLC films in relation to the substrate bias voltage (Vs). films are compared with those of the OLC films. A high purity sintered graphite target was mounted on a cathode as a carbon source. Nitrogen or argon was introduced into a deposition chamber through each mass flow controller. After the initiation of an arc plasma at 60 A and 1 Pa, the target surface was heated and evaporated by the plasma. Carbon atoms and clusters evaporated from the target were ionized partially and reacted with activated nitrogen species, and a carbon nitride film was deposited onto a Si (100) substrate when we used nitrogen as a reactant gas. The surface of the growing film also reacted with activated nitrogen species. Carbon macropartic1es (0.1 -100 maicro-m) evaporated from the target at the same time were not ionized and did not react fully with nitrogen species. These macroparticles interfered with the formation of the carbon nitride film. Therefore we set a shielding plate made of stainless steel between the target and the substrate to trap the macropartic1es. This shielding method is very effective to prepare smooth a-CN films. We, therefore, call this method "shielded arc ion plating (SAIP)". For the deposition of DLC films we used argon instead of nitrogen. Films of about 150 nm in thickness were deposited onto Si substrates. Their structures, chemical compositions and chemical bonding states were analyzed by using X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and infrared spectroscopy. Hardness of the films was measured with a nanointender interfaced with an atomic force microscope (AFM). A Berkovich-type diamond tip whose radius was less than 100 nm was used for the measurement. A force-displacement curve of each film was measured at a peak load force of 250 maicro-N. Load, hold and unload times for each indentation were 2.5, 0 and 2.5 s, respectively. Hardness of each film was determined from five force-displacement curves. Wear resistance of the films was analyzed as follows. First, each film surface was scanned with the diamond tip at a constant load force of 20 maicro-N. The tip scanning was repeated 30 times in a 1 urn-square region with 512 lines at a scanning rate of 2 um/ s. After this tip-scanning, the film surface was observed in the AFM mode at a constant force of 5 maicro-N with the same Berkovich-type tip. The hardness of a-CN films was less dependent on Vs. The hardness of the film deposited at Vs=O V in a nitrogen plasma was about 10 GPa and almost similar to that of Si. It slightly increased to 12 - 15 GPa when a bias voltage of -100 - -500 V was applied to the substrate with showing its maximum at Vs=-300 V. The film deposited at Vs=O V was least wear resistant which was consistent with its lowest hardness. The biased films became more wear resistant. Particularly the film deposited at Vs=-300 V showed remarkable wear resistance. Its wear depth was too shallow to be measured with AFM. On the other hand, the DLC film, deposited at Vs=-l00 V in an argon plasma, whose hardness was 35 GPa was obviously worn under the same wear test conditions. The a-C:N films show higher wear resistance than DLC films and are useful for wear resistant coatings on various mechanical and electronic parts.nic parts.
Kim, Dong-Hwan;Bae, Ji-Hyun;Cho, Byeong-Hoon;Lee, In-Bog;Baek, Seung-Ho;Ryu, Hyun-Mi;Son, Ho-Hyun;Um, Chung-Moon;Kwon, Hyuck-Choon
Restorative Dentistry and Endodontics
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v.29
no.2
/
pp.170-176
/
2004
Objectives : In the unique metal iris method. the developing interfacial gap at the cavity floor resulting from the cavity wall property during polymerizing composite resin might affect the nominal shear bond strength values. The aim of this study is to evaluate that the iris method reduces the cohesive failure in the substrates and the cavity wall property effects on the shear bond strength tests using iris method. Materials and Methods : The occlusal dentin of 64 extracted human molars were randomly divided into 4 groups to simulate two different levels of cavity wall property (metal and dentin iris) and two different materials ($ONE-STEP^{\circledR}$ and $ALL-BOND^{\circledR}$ 2) for each wall property. After positioning the iris on the dentin surface. composite resin was packed and light-cured. After 24 hours the shear bond strength was measured at a crosshead speed of 0.5 mm/min. Fracture analysis was performed using a microscope and SEM. The data was analyzed statistically by a two-way ANOV A and t-test. Results : The shear bond strength with metal iris was significant higher than those with dentin iris (p=0.034). Using $ONE-STEP^{\circledR}$, the shear bond strength with metal iris was significant higher than those with dentin iris (p=0.005), but not in $ALL-BOND^{\circledR}$ 2 (p=0.774). The incidence of cohesive failure was very lower than other shear bond strength tests that did not use iris method. Conclusions:The iris method may significantly reduce the cohesive failures in the substrates. According to the bonding agent systems. the shear bond strength was affected by the cavity wall property.
A simultaneous official method was developed for the determination of phorate and its metabolites (phorate sulfoxide, phorate sulfone, phorate oxon, phorate oxon sulfoxide, phorate oxon sulfone) in livestock samples. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Phorate and its metabolites were extracted from beef and milk samples with acidified acetonitrile (containing 1% acetic acid) and partitioned with anhydrous magnesium sulfate. Then, the extract was purified through primary secondary amine (PSA) and C18 dispersive sorbent. Matrix matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/L) for all the analytes into blank extract with $r^2$ > 0.996. For validation purposes, recovery studies were carried out at three different concentration levels (beef 0.004, 0.04 and 0.2 mg/kg; milk 0.008, 0.04 and 0.2 mg/kg, n = 5). The recoveries were within 79.2-113.9% with relative standard deviations (RSDs) less than 19.2% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines. The limit of quantification was quite lower than the maximum residue limit (MRL) set by the Ministry of Food and Drug Safety (0.05 mg/kg). The proposed analytical method was accurate, effective and sensitive for phorate and its metabolites determination and it will be used to as an official analytical method in Korea.
17β-estradiol (E2) is a natural hormone secreted by ovary, and continuously discharged from household and livestock wastewater into aquatic environment. Due to its strong estrogenic activity, it has adverse effects on development and reproduction in crustacean as an endocrine disrupting chemical. Although ecdysteroid signaling pathway play a key role in development in crustacean, little information on transcriptional modulation of ecdysteroid-related genes in response to E2 is available in small crustacean. Here, we investigated the acute toxicity of E2 to obtain 24-h LCx values in the brackish water flea Diaphanosoma celebensis. Time-dependent expression patterns of seven ecdysteroid pathway - related genes (CYP314a1, EcRA, EcRB, USP, ERR, Vtg, VtgR) were further examined using quantitative real time reverse transcriptase polymerase chain reaction (qRT-PCR). As results, 24-h LC50 and LC10 values were 9.581 mg/l and 4.842 mg/l, respectively. The mRNA expression of CYP314a1, EcRA, USP, VtgR was significantly up-regulated at 12 or 24 h after exposure to E2. These findings indicate that E2 can affect their molting and reproduction by modulating the expression of ecdysteroid pathway - related in D. celebensis. This study will be useful for better understanding of molecular mode of action of endocrine disrupting chemicals on molting process in small crustacean.
Gu, Sun Young;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Lee, Jung Mi;Jung, Yong-hyun;Moon, Guiim
Korean Journal of Environmental Agriculture
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v.41
no.2
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pp.82-94
/
2022
BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.
Damages by heavy snow does not occur very often, but when it does, it causes damage to a wide area. To mitigate snow damage, it is necessary to know, in advance, the depth of snow that causes damage in each region. However, snow depths are measured at observatory locations, and it is difficult to understand the spatial distribution of snow depth that causes damage in a region. To understand the spatial distribution of snow depth, the point measurements are interpolated. However, estimating spatial distribution of snow depth is not easy when the number of measured snow depth is small and topographical characteristics such as altitude are not similar. To overcome this limit, satellite images such as Synthetic Aperture Radar (SAR) can be analyzed using Differential Interferometric SAR (DInSAR) method. DInSAR uses two different SAR images measured at two different times, and is generally used to track minor changes in topography. In this study, the spatial distribution of snow depth was estimated by DInSAR analysis using dual polarimetric IW mode C-band SAR data of Sentinel-1B satellite operated by the European Space Agency (ESA). In addition, snow depth was estimated using geostationary satellite Chollian-2 (GK-2A) to compare with the snow depth from DInSAR method. As a result, the accuracy of snow cover estimation in terms with grids was about 0.92% for DInSAR and about 0.71% for GK-2A, indicating high applicability of DInSAR method. Although there were cases of overestimation of the snow depth, sufficient information was provided for estimating the spatial distribution of the snow depth. And this will be helpful in understanding regional damage-causing snow depth.
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