The purpose of this study was to investigate the changes of taste components in the boiled beef brisket soup stock and shank soup stock by varying pretreatment, boiling temperature and time. Free amino acids and nucleotides color and sensory evaluation in each samples were analyzed. The results were obtained as follows : 1. The amount of free amino acids in the brisket soup stock pretreated by soaking and blanching showed a tendency to increase in proportion to boiling time. The amount of glutamic acid in the brisket soup stock was much in order of soaking > blanching > roasting pretreatment. While the amount of glutamic acid in the boiled soup stock samples pretreated by soaking and blanching was much more at low temperature than at high temperature, the glutamic acid contents in the boiled soup stock pretreated by roasting were large at high temperature. The amount of glutamic acid in pretreated by soaked soup stock showed the highest and recorded 8.73 mg% at 6 hour-low temperature-boiling. 2. The amount of free amino acids in the shank soup stock did not show any regular tendency and had few changes in quantity by the methods of pretreatment. Each amount of glutamic acid in the shank soup stock pretreated by soaking and blanching was the highest, when boiled for 3 hours at high temperature. The samples pretreated by roasting showed the highest record 2.49 mg%, when boiled for 6 hours at high temperature, but could not recognize any regular tendency in the case of boiling at low temperature. 3. The amount of nucleotides in the brisket soup stock generally showed increase in proportion to boiling time. The amount of 5'-IMP extracted from the brisket soup stock was much in order of blanching > soaking > roaking pretreatment, but few differences between blanching and soaking soup stock samples. The amount of 5'-IMP extracted from soup stock samples pretreated by soaking and blanching was high at low-boiling and by roasting at high-boiling. Each amount of 5'-IMP extracted from soup stocks pretreated by soaking(BSL) and blanching(BBL) was the highest at 6 hour-low-boiling(37.06 mg%), and 5 hours(38.37 mg%) respectively. The amount of 5'in the soup stock pretreated by roasting(BRH) showed the highest records at 6 hour-high-boiling(10.85 mg%). 4. The amount of 5'-IMP extracted from the shank soup stock preteated by soaking and blanching showed a tendency to decrease after 3 hours boiling irrelative of boiling temperature. The amount of 5'in the shank soup stock was much in order of soaking > blanching > roasting pretreatment and showed high at the boiling of high temperature. In the sample pretreated by roasting it showed the highst records when boiled for 6 hours at high temperature(1.55 mg%). 5. The L Value of the brisket soup stock pretreared by roasting at high temperature(BRH) was the lowest and the b value of it was the highest of all the brisket samples boiled for 6 hours. No differences were found in the Value of L, a, and b in shank soup stock by the methods of pretreatment and boiling temperature. 6. The sensory scores in color and flavor of the brisket soup stock showd that BRH was higher than the other samples, and the preference in taste and overall was the highest in BSH while it was the lowest in BRH. The preference in the all sensory characteristics of SSH was higher than any other shank soup stock, but did not show any significant difference statistically.
This study was conducted to evaluate two sample digestion procedures and instrumental determination parameters for analysis of lead in bone. Amputated human legs were treated by acid digestion or microwave dissolution prior to spectrometric analysis. Inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS) were used for determining bone lead levels. Recovery efficiencies using standard reference material from acid digestion measured by ICP-MS were in good agreement with those of the certified value, but in cases of acid digestion by GF-AAS and microwave digestion by both two methods, recovery underestimated and overestimated, respectively. For the bone samples, the lead concentrations obtained by ICP-MS after acid digestionwere in good agreement with those by GF-AAS (correlation coefficient = 0.983), but GF-AAS gave systematically higher values than ICP-MS. While a good agreement between two analytical methods after microwave digestion was also obtained (correlation coefficient = 0.950), bone lead concentrations from microwave were relatively higher than those from acid digestion. In conclusion, the use of the simple nitric acid digestion procedure at an ambient temperature coupled to ICP-MS seems to be efficient for the determination of lead in bone in consideration for both the convenience and validity.
The purpose of this study was to evaluate and compare the shear bond strength of orthodontic brackets depending on the variety of adhesives and whether saliva exists, by using self-etching primer (SEP). Groups were divided according to the type of adhesive into resin adhesive (Trans bond XT) and resin-modified glass ionomer cement (Fuji Ortho LC). One group of resin adhesive used XT primer after etching with 37% phosphoric acid, and the other group used self-etching primer. One group of resin-modified glass ionomer cement only used etching for bonding, and the other group used SEP. Each of the groups were also classified by whether saliva was contaminated or not. and then the shear bond strength was measured. The results showed that when using resin adhesive, the shear bond strength of SEP was lower than the XT primer. In the resin-modified glass ionomer cement groups, the shear bond strength which depends on the priming method, did not have a meaningful difference statistically When saliva was contaminated, the group which used SEP, regardless of the adhesive variety, had a greater shear bond strength than the normal priming group. From these results, SEP showed a shear bond strength that is possible to be used clinically, regardless of the adhesive variety. It can especially be clinically useful to use SEP to bond brackets even on tooth surfaces contaminated with saliva, because it offers the appropriate bonding strength as well as shorter treatment time and easy application.
Cyantraniliprole, which is an ananthranilic diamide insecticide that was developed by the DuPont Corporation, was registered in the Republic of Korea in 2012. It offers exceptional insecticidal activity on a broad range of Lepidopera, Coleoptera, Diptera, and Isoptera. The maximum residue limits are set to pepper, peach, apple, sweet pepper, welsh onion, and so on (0.2~2.0 mg/kg). Therefore, an analytical method for determining cyantraniliprole residue in agricultural products was developed to ensure food safety. In previous studies, welsh onions were among vegetables included in the allium species, which is a representative plant with sulfur organic compounds. In this study, the analytical method was developed and evaluated for the elimination of sulfur compounds from the test solution of allium species during pesticide residue analysis. In order to inactivate the enzyme allinase and produce sulfur compounds, sample extraction was made in the base state pH 10 by reducing the activity of the enzyme. The recoveries of the developed method ranged from 81.9% to 83.2%, and the relative standard deviations were less than 10%. Therefore, based on the results, the method developed in this study is accurate and appropriate for use in cyantraniliprole determination. It will be used as the official method for managing the safety of cyantraniliprole residues in agricultural products.
Lee, Hyo Sub;Hong, Su Myeong;Kim, Taek Kyum;Kwon, Hye Young;Kim, Dan Bi;Moon, Byeong Chul;Moon, Joon Kwan
The Korean Journal of Pesticide Science
/
v.20
no.4
/
pp.312-318
/
2016
This study investigated the reduction of residual pesticide in soil by using eight kinds of soil amendments such as shell, quick lime, dolomite, silicic acid, leaf mold, oil cake, bed soil and husk. A total of ten pesticides most frequently detected in agricultural soil were selected (azoxystrobin etc.) and soil amendments were treated in soils at a 2% application rate and incubated for 7 days. Pesticides were analyzed by HPLC-MS/MS with QuEChERS-based sample preparation procedure and pH was measured on 1, 3 and 7 days. This study showed that, soil amemdments were effective in reducing pesticides after 7days of incubation. Over 90% of azoxystrobin, cadusafos, chlorpyrifos, fluquinconazole, imidacloprid, isoprothiolane and procymidone were decomposed from soils amended with 2% quick lime, whereas the concentration of boscalid, dimethomorph and triycyclazole were not decreased. The soil pH increased to 12.8-12.9 in soil amended with quick lime, but other soil conditioners did not change the soil pH. Quick lime was particularly effective in reducing residual pesticides.
The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.
The determination of phthalates and adipate in natural mineral water and its container is described. Phthalates and adipate were extracted from natural mineral water by liquid-liquid extraction with methylene chloride, concentrated and then injected in GC-MS (SIM). Phthalates and adipate from 1) PET, cap, label and glue were extracted in Soxhlet with 50 mL of carbon tetrachloride, purified with silicagel and detected with GC-MS (SIM). Peak shapes and quantitation of phthalates and adipate were excellent, with linear calibration curves over a range of $0.1{\sim}10{\mu}g/L$ in water sample ($r^2$ > 0.996) and over a range of $1{\sim}1,000{\mu}g/Kg$ in solid samples ($r^2$>0.994). The detection limits of analytes were $0.002{\sim}0.010{\mu}g/L$ in water and $0.01{\sim}0.02{\mu}g/Kg$ in solid samples. Five kinds of natural mineral water samples, two PETs, two labels, two caps and two glues were quantified by the described procedure. As a results, the concentrations of total phthalates in natural mineral water ranged from ND ~ 1.2 ng/mL. Otherwise, the concentrations of total phthalate extracted from PET ranged from 0.55 ~ 1.2 mg/Kg. We found that the accurate determination of phthalte and adipate in natural mineral water and container must be considered blank correction and the removal of label and glue in PET sample.
Tetracycline antibiotics have been widely used not only therapeutics but feed additives. There are many methods for the isolation and determination of tetracycline antibiotics in animal muscle tissue. But those methods take much time and labor, so it is difficult to analyse many samples simultaneously. A rapid isolation method and liquid chromatographic determination of tetracycline antibiotics in animal muscle tissue (bovine, porcine, chicken) is presented. Blank control and tetracyclines fortified samples (0.5g) were blended with $C_{18}$ containing 0.05g each of oxalic acid and disodium ethylenediaminetetraacetate. After homogenize, homogenate was transferred to glass column made from 10ml glass syringe and compressed to 4~4.5ml volume. A column made from the $C_{18}$/meat matrix was washed with hexane (8ml) and dichloromethane (8ml, if needed), following which the tetracyclines were eluted,vith methanol or 0.01M methanolic oxalic acid (8ml). The eluates containing tetracyclines analytes were free from interfering compounds when analysed by HPLC with UV detection (photodiode array at 360nm). Standard curve for each tetracycline showed a linear response at the range of $0.05{\sim}1.0{\mu}g/ml$ and tetracycline antibiotics were eluted within 4ml of eluted volume. All tetracycline antibiotics except tetracycline were stable during the concentration process at $40^{\circ}C$ and time required for concentration was 3~4 hours. Fortified samples containing oxalic aicd and EDTA represented more good recoveries than those of not-contained sample. Recoveries were 91.8~110.1% (oxytetracycline; OTC), 57.7~79.5% (tetracycline; TC), 78.1~88.6% (chlortetracyclines; CTC) and 88.4~100.6% (doxycycline; DC) in pork tissue, 101.1~126.8% (OTC), 66.4~75.4% (TC), 79.2~88.1% (CTC) and 69.3~86.7% (DC) in beef tissue, and 90.8~95.6% (OTC), 66.2~84.4% (TC), 75.7~77.2% (CTC) and 55.6~80.7% (DC) in chicken muscle tissue. The detection limits validated in muscle tissue by this method were $0.05{\mu}g/g$ for OTC and TC, and $0.1{\mu}g/g$ for CTC and DC.
An advanced extraction method by ultrasonic extraction with applied solid phase extraction (SPE) has been developed for the determination of simultaneous eight major ginsenosides, namely ginsenosides Rg1, Re, Rf, Rb1, Rg2, Rc, Rb2, and Rd in the root of Panax ginseng. Four extraction methods including n-BuOH reflux extraction (Method A), 70% EtOH reflux extraction (Method B), 50% MeOH reflux extraction with SPE (Method C), and 50% MeOH ultrasonication with SPE clean-up process (Method D) were investigated for the determination of eight major ginsenosides. Total contents of ginsenosides were highest by extraction of Method C as $2.408{\pm}0.011%$. However, Method D was evaluated as relatively simpler and more efficient method due to short extraction time, small solvent consumption and less expensive, compared to conservative reflux method. Ginsenosides were also satisfactorily separated with good resolution and the accuracy range was between 1.05 and 4.06% as relative standard deviation (RSD) by Method D. SPE condition and HPLC condition were further optimized for determination of eight major ginsenosides by the ultrasonic extraction method. Conclusively, ultrasonic extraction of 2 g sample of ginseng using ultrasonic bath and 1 loading for SPE was evaluated as proper condition for extraction of ginseng.
Sensitive and specific monoclonal antibody (MAb) was produced from hybridoma (1H11-5) obtained by fusion of myeloma cell (V653) and spleen cell isolated from mouse immunized sulfamthazine (SMZ)-HG-KLH. Direct competitive ELISA was developed for rapid detection of SMZ in milk samples using MAb against SMZ with optimized conditions between MAb and SMZ-HG-HRP conjugate, and applicable conditions for analysis of milk samples were established. Detection range of immunoassay was 0.1 to 100 ppb. Recoveries from spiked raw milk and processed milk samples averaged 82.1-120.7 and 82.1-97.1%, respectively.
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