Unsaponifiables in the kernel and the cob of 7 maize varieties were analyzed by using thin-layer chromatography (TLC) and gas chromatography (GC) for the identification of phytosterols and their concentrations. The unsaponifiables of the kernel were clearly separated into band I (campesterol, stigmasterol, and ${\beta}$-sitosterol), band II (${\Delta}^5$-avenasterol), band III (${\Delta}^7$- stigmastenol), and band IV (${\Delta}^7$-avenasterol). In the cob, on the other hand, three or more bands were separated in addition to bands. The GC analysis of unsaponifiables showed good separation of campesterol, stigmasterol and ${\beta}$-sitosterol, but the mixture of ${\Delta}^7$-avenasterol (retention time[RT] 22.846), ${\Delta}^7$-stigmastenol (RT 22.852), and ${\Delta}^5$-avenasterol (RT 22.862) showed poor separation. Phytosterol content of the maize kernel was 635.9 mg/100 g, and that of the cob was 273.0 mg/100 g, respectively. The phytosterol content of the kernel was 2.4-fold higher than that of the cob. The phytosterol content of the kernel was higher in the order ${\beta}$sitosterol 80.05% > campesterol 10.5% > stigmasterol 9.46%, but that of the cob was higher in the order ${\beta}$-sitosterol 59.43% > stigmasterol 31.72% > campesterol 10.98%. Based on these results, it appears that the phytosterols of the maize kernel are synthesized in the maize cob and are transferred to the kernel, because the precursors (${\Delta}^7$-avenasterol, ${\Delta}^7$-stigmastenol, and ${\Delta}^5$-avenasterol) of major phytosterols were detected in maize cobs.
In this study, the hydrochemical and the isotopic characteristics of major streams in the Daejeon area were investigated during rainy and dry seasons. The stream water shows the electrical conductivity of the range of $37{\sim}527{\mu}s$/cm, and pH $6.21{\sim}9.83$. The chemical composition of stream waters can be grouped as three types: the upper streams of Ca(Mg)-$HCO_3$ type, Ca(Mg)-$SO_4(Cl)$ type of middle streams flowing through urban area, and Na(Ca)-$HCO_3$(Cl, $SO_4$) type of the down streams. Based on in-situ investigation, the high pH of stream waters flowing through urban area is likely to be caused by the inflow of a synthetic detergent discharging from the apartment complex. The electrical conductivity of stream waters at a dry season is higher than those of at a rainy season. We suggest that the hydro-chemical composition of stream waters in the Daejeon area was affected by the discharging water from the sewage treatment facilities and anthropogenic contaminants as well as the interaction with soil and rocks. ${\delta}D$ and ${\delta}^{18}O$ values of the stream waters show the relationship of ${\delta}D=6.45{\delta}^{18}O-7.4$, which is plotted at a lower area than global meteoric water line(GMWL) of Craig(1961). It is likely that this isotopic range results from the evaporation effect of stram waters and the change of an air mass. The isotope value shows an increasing trend from upper stream to lower stream, that reflects the isotopic altitude effect. The relationship between ${\delta}^{13}C$ and $EpCO_2$ indicates that the carbon as bicarbonate in stream water is mainly originated from $CO_2$ in the air and organic materials. The increasing trend of ${\delta}^{13}C$ value from upper stream waters to lower stream waters can be attributed to the following reasons: (1) an increasing dissolution of $CO_2$ gas from a contaminated air in downtown area of the Daejeon, and (2) the increment of an inorganic carbon of groundwater inflowed into stream by base flow. Based on the relationship between ${\delta}^{34}S$ and $SO_4$ of stream waters, the stream waters can be divided into four groups. $SO_4$ content increases as a following order: upper and middle Gab stream${\delta}^{34}S$ value decreases as above order. ${\delta}^{34}S$ value indicates that sulfur of stream waters is mainly originated from atmosphere, and is additionally supplied by pyrite source according to the increase of sulfate content. The sulfur isotope analysis of a synthetic detergent and sewage water as a potential source of the sulfur in stream waters is furtherly needed.
BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.
The method for the determination of ethylenediamine (EDA) and hexamethylenediamine (HMDA) in food simulants was developed, and migration amounts of these compounds was monitored for 124 polyamide (PA) utensils. The diurethane derivatives of EDA and HMDA, which produced by reaction with ethyl chloroformate, were analyzed by using gas chromatograph (GC)/flame ionization detector (FID) and GC/mass spectrometer (MS). The developed method was validated with $0.3\;{\mu}g/mL$ of limit of detection (LOD) for EDA and $0.1\;{\mu}g/mL$ of LOD for HMDA, > 0.999 of linearity($r^2$) and > 88% of recovery. The EDA was detected 1.31 and $02.06\;{\mu}g/mL$ for 2 samples in water. The HMDA was detected $0.29\;-\;0.93\;{\mu}g/mL$ for 3 samples in 20% ethanol and $0.26\;-\;0.44\;{\mu}g/mL$ for 10 samples in n-heptane. These migration levels were below the specific migration limits (SML) of $12\;{\mu}g/mL$ and $2.4\;{\mu}g/mL$ for EDA and HMDA established in EU.
Choi, Seung-Hyun;Kim, Jae-Min;Choi, Sun-il;Jung, Tae-Dong;Cho, Bong-Yeon;Lee, Jin-Ha;Lee, Gunyoung;Lim, Ho Soo;Yun, Sang Soon;Lee, Ok-Hwan
Journal of Food Hygiene and Safety
/
v.32
no.4
/
pp.284-289
/
2017
Oxidized polyethylene wax (OPEW) is, one of the food additives, used as a coating agent in citrus fruits and nuts. OPEW is authorized to quantum satis in EU, USA, and is acceptable less than 250 mg/kg in Australia and New Zealand. But OPEW is unauthorized as a food additive in Korea. This study was to establish the analytical method of OPEW and demonstrate the effective application of various food samples. We first conducted to compare the various analytical method including acid value (AV), high temperature gel permeation chromatography (HT-GPC), matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF/MS), gas chromatography flame ionization detector (GC-FID) and fourier transform infrared spectroscopy (FT-IR). This result indicated that FT-IR spectrum of OPEW treated food sample displayed absorption bands for carbonyl group (C=O, $1714cm^{-1}$), ester group (C-O, $1463cm^{-1}$), aliphatic group (C-H, $2916cm^{-1}$). Furthermore, IR spectrum of OPEW treated food sample showed similar tendency with IR spectrum of OPEW standard. Therefore, it is confirmed that analytical method using FT-IR can be detected on analysis of OPEW in food. As a result of monitoring of 111 samples using established analytical method, OPEW was not detected in the food samples.
The Seongsan mine is one of the largest dickite deposits in the southwestern part of the Korean Peninsula. The main constithent minerals of the ore are dickite and quartz with accessory alunite, kaolinite and sericite. The geology around the Seongsan mine consists mainly of the late Cretaceous felsic volcanic rocks. In the studied area, these rocks make a synclinal structure with an axis of E-W direction plunging to the east. Most of the felsic volcanic rocks have undergone extensive hydrothermal alteration. The hydrothermally altered rocks can be classified into the following zones: Dickite, Dickite-Quartz, Quartz, Sericite, Albite and Chlorite zones, from the center to the margin of the alteration mass. Such zonal arrangement of altered rocks suggests that the country rocks, most of which are upper part of the rhyolite and welded tuff, were altered by strongly acid hydrothermal solutions. It is reasonable to consider that initial gas and solution containing $H_2S$ and other compounds were oxidized near the surface, and formed hydrothermal sulfuric acid solutions. The mineralogical and chemical changes of the altered rocks were investigated using various methods, and chemical composition of fifty-six samples of the altered rocks were obtained by wet chemical analysis and X.R.F. methods. On the basis of these analyses, it was found that some components such as $SiO_2$, $Al_2O_3$, $Fe_2O_3$, CaO, MgO, $K_2O$, $Na_2O$ and $TiO_2$ were mobilized considerably from the original rocks. The formation temperature of the deposits was estimated as higher than $200^{\circ}C$ from fluid inclusion study of samples taken from the Quartz zone. On the basis of the chemical composition data on rocks and minerals and estimated temperatures, the hydrothermal solutions responsible for the formation of the Seongsan dickite deposits were estimated to have the composition: $m_{K^+}=0.003$, $m_{Na^+}=0.097$, $m_{SiO_2(aq.)}=0.008$ and pH=5.0, here "m" represents the molality (mole/kg $H_2O$).
Background : Secondary pulmonary hypertension is an important final endpoint in patients with chronic hypoxic lung disease, accompanied by deterioration of pulmonary hemodynamics. The clinical diagnosis of pulmonary hypertension and/or cor pulmonale could be difficult, and simple noninvasive evaluation of pulmonary artery pressures has been an relevant clinical challenge for many years. Doppler echocardiography might to be a more reliable method for evaluating pulmonary hemodynamics in such patients in terms of the accuracy, reproducibility and easiness for obtaining an appropriate echocardiographic window than M-mode echocardiography. The aim of this study was to assess echocardiographic parameters associated with pulmonary arterial hypertension, defined by increasing right ventricular systolic pressure(RVSP), calculated from trans-tricuspid gradient in patients with chronic hypoxic lungs. Method : We examined 19 patients with chronic hypoxic lung disease, suspected pulmonary hypertension under the clinical guidelines by two dimensional echocardiography via the left parasternal and subcostal approach in a supine position. Doppler echocardiography measured RVSP from tricuspid regurgitant velocity in continuous wave with 2.5MHz transducer and acceleration time(AT) on right ventricular outflow tract in pulsed wave for the estimation of pulmonary arterial pressure. Results : On echocardiography, moderate to severe degree of pulmonary arterial hypertension was defined as RVSP more than 40mmHg, presenting tricuspid regurgitation. Increased right ventricular endsystolic diameter and shortened AT were noted in the increased RVSP group. Increased RVSP was correlated negatively with the shortening of AT. Other clinical data, including pulmonary functional parameters, arterial blood gas analysis and M mode echocardiographic parameters were not changed significantly with the increased RVSP. Conclusion : These findings suggest that shortened AT on pulsed doppler can be useful when quantifying pulmonary arterial pressure with increased RVSP in patients with chronic lung disease with hypoxemia. Doppler echocardiography in pulmonary hypertension of chronic hypoxic lungs is an useful option, based on noninvasiveness under routine clinical practice.
The cardiopulmonary and antagonistic effects of atipamezole, to medetomidine (30 ug/kg, IM)-tiletamine/zolazepam (10 mg/kg, IV) were determined. Twelve healthy mongrel dogs ,(4.00$\pm$0.53 kg, mean$\pm$SD) were randomly assigned to the four experimental groups (control, A30; atipamezole 30 ug/kg, A60; atipamezole 60 ug/kg, A150; atipamezole 150 ug/kg) with 3 dogs in each group. Atropine (0.03 mg/kg, IM), medetomidine, and tiletamine/zolazepam (TZ) were injected 10 minute intervals. Atipamezole was injected intravenously 15 minutes after TZ injection. Mean arousal time (MAT) was 52.50$\pm$4.98, 43.06$\pm$2.60, 32.83$\pm$8.13, and 14.36$\pm$1.60 minutes in control, A30, A60, and Al50 groups respectively. In Al50 group, MAT was significantly reduced (P < 0.05). but mean walking time (MWT) was similar to that in control group. In recovery period, the higher doses of atimapezole, the rougher recovery including head rocking, hypersalivation, and muscle twitching. Five of twelve dogs vomited within 5 minutes after medetomidine injection. In Control group, heart rate significantly decreased in all recording stages except 15 minutes after TZ injection, 10 minutes after medetomidine injection in all groups, and 40 minutes after atipamezole injection in A30 group (P < 0.05). In Al50 group, atipamezole reversed the respiratory depression induced by medetomidine. Arterial blood pressure was significantly decreased 10minutes after medetomidine injection and 15 minutes after TZ injection in almost dogs in this study (P < 0.05). From 10 minutes after atipamezole injection to arousal time, arterial blood pressure was progressively increased in A60 and A150 group. Any value of blood gas analysis and CBC, and serum chemistry values were not significantly changed except pH of Al50 at 10 minutes after medetomidine injection. As shown in present study, atipamezole(150 ug/kg) is considered to exert a useful reversal effect in dogs anesthetized with medetomidine-tiletamine/zolazepam combination.
The changes in the volatile organic compounds in plum after its electron beam irradiation and storage were determined using the simultaneous distillation extraction method and gas chromatograph-mass spectrometry. There were 44, 46, 45, 47, and 38 volatile compounds in the 0-, 0.25-, 0.5-, 0.75-, and 1 kGy irradiated samples, respectively. Also, the volatile flavor components of the plum that was stored for 30 days were identified as 48, 40, 40, 39, and 40 components. The compositions of the volatile compounds of the control and irradiated samples showed a similarity after the storage. Especially, the more important volatile flavor of the plum was identified as hexanal of the C6compounds, (E)-2-hexenal and (Z)-3-hexenal. In particular, hexanal, (E)-2-hexenal, and (Z)-3-hexen-1-ol increased in all the doses, where as hexanol and (E)-2-hexen-1-ol decreased. Among the lactone compounds, ${\gamma}$-hexalactone, ${\gamma}$-octalactone, and ${\gamma}$-decalactone were identified during the storage period in the raw samples. Hexanonic acid and 2-hexenoic acid were not identified during the storage of the samples, and 2-methylprrole was detected only when the storage samples were irradiated at a dose higher than 0.5kGy. Therefore, it was shown that there was no effect on the variation of the volatile organic component suntil 1 kGy in the plum was irradiated with an electron beam.
Kim, Hea Na;Kim, Seong Beom;Choi, Eun;Woo, Min Ji;Kim, Ji Yoon;Saravanan, Manoharan;Hur, Jang Hyun
The Korean Journal of Pesticide Science
/
v.18
no.3
/
pp.123-129
/
2014
The present work was aimed to determine the pre-harvest residue limits (PHRLs) and the safety management of commonly used pesticides namely buprofezin and penthiopyrad on oriental melon (Cucumis melon var. makuwa). In this study, the buprofezin (diluted two thousand fold) and penthiopyrad (diluted four thousand fold) were sprayed single time on oriental melon in the cultivation areas Sangju (site 1) and Sungju (site 2). Oriental melon were randomly collected from the both areas at the end of 0 (2 hours after pesticides spaying), 1, 2, 3, 5, 7, 9 and 10 days. For analysis, each samples were partitioned twice (80 and 70 mL) with dichloromethane and purified by florisil SPE cartridge. Finally, the residual amounts of both pesticides in all samples were analyzed using gas chromatography/nitrogen phosphorus detector (GC/NPD). In this study, the method limit of quantification (MLOQ) for both buprofezin and penthiopyrad in oriental melon was found to be $0.01mg\;kg^{-1}$ and their recovery levels were 91.1~98.6% and 90.0~104.6%, respectively. Further, the calculated biological half-life for buprofezin and penthiopyrad in oriental melon were 3.9 and 3.5, and 3.0 and 2.7 days in site 1 and 2, respectively. The results of this study found that the PHRLs for buprofezin and penthiopyrad were 4.24 and $2.31mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggest that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when oriental melon is harvested.
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