Purpose: We established radiolabeling conditions of NOTA and DOTA with a generator-produced PET radionuclide $^{68}$Ga and studied in vitro characteristics such as stability, serum protein binding, octanol/water distribution, and interference with other metal ions. Materials and Methods: Various concentrations of NOTA 3HCl and DOTA 4HCl were labeled with 1 mL $^{68}$GaCl$_3$ (0.18$\sim$5.75 mCi in 0.1 M HCl in various pH. NOTA 3HCl (0.373 mM) was labeled with $^{68}$GaCl$_3$(0.183$\sim$0.232 mCi/0.1 M HCl 1.0 mL) in the presence of CuCl$_2$, FeCl$_2$, InCl$_3$, FeCl$_3$, GaCl$_3$, MgCl$_2$ or CaCl$_2$ (0$\sim$6.07 mM) at room temperature. The labeling efficiencies of $^{68}$Ga-NOTA and $^{68}$Ga-DOTA were checked by ITLC-SG using acetone or saline as mobile phase. Stabilities, protein bindings, and octanol distribution coefficients of the labeled compounds also were investigated. Results: $^{68}$Ga-NOTA and $^{68}$Ga-DOTA were labeled optimally at pH 6.5 and pH 3.5, respectively, and the chelates were stable for 4 hr either in the reaction mixture at room temperature or in the human serum at 37$^{\circ}C$. NOTA was labeled at room temperature while DOTA required heating for labeling. $^{68}$Ga-NOTA labeling efficiency was reduced by CuCl$_2$, FeCl$_2$, InCl$_2$, FeCl$_3$ or CaCl$_3$, however, was not influenced by MgCl$_2$ or CaCl$_2$. The protein binding was low (2.04$\sim$3.32%). Log P value of $^{68}$Ga-NOTA was -3.07 indicating high hydrophilicity. Conclusion: We found that NOTA is a better bifunctional chelating agent than DOTA for $^{68}$Ga labeling. Although, $^{68}$Ga-NOTA labeling is interfered by various metal ions, it shows high stability and low serum protein binding.
Hwang, Kyung Mi;Ham, Hyeon Suk;Lee, Hwa Jung;Kang, Yoon Jung;Yoon, Hae Seong;Hong, Jin Hwan;Lee, Hyoun Young;Kim, Cheon Hoe;Oh, Keum Soon
Journal of Food Hygiene and Safety
/
v.32
no.5
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pp.411-417
/
2017
This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.
It was carried out to detect anti-impotence drug-like compounds, sibutramine and their analogues in dietary supplements, which are doubtful whether they include illegal compounds. A total of 51 food products were bought online and have been investigated. The separation was achieved on a C18 column, with the mobile phase made up of water (5 mM sodium hexanesulfonate and 0.1% phosphoric acid) and 95% acetonitrile, at a flow rate of 1.2 mL/min with gradient elution using by HPLC-DAD. The UV signals were monitored at 220 nm and 291 nm. LC-ESI-tandom MS was utilized to confirm that detected compounds in samples are the same as the reference materials. Two nutrient supplement foods and ginseng products were found to contain 1.3-82.1 mg of sildenafil, dimethylthiolsildenafil and pseudovardenafil per serving size. In addition, two other processed products were detected to contain 1.7 and 2.2 mg of didesmethylsibutramine, derived from sibutramine per serving size.
Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
Korean Journal of Food Science and Technology
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v.44
no.3
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pp.263-268
/
2012
Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.
Na, Hwan Sik;Kim, Jin Young;Yun, Seol Hee;Park, Hak Jae;Choi, Gyeong Cheol;Yang, Soo In;Lee, Ji Heon;Cho, Jeong Young
Food Science and Preservation
/
v.20
no.4
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pp.451-458
/
2013
The purpose of this research is to distinguish the quantitative determination of phytochemicals in various agricultural products and to optimize an HPLC method for the determination of lycopene, lutein, ${\alpha}$-carotene, ${\beta}$-carotene, and cryptoxanthin. Among the different conditions studied, the most suitable ones for our samples were the extraction with hexane/acetone/ethanol (50:25:25, v/v/v), dissolution of the dry extract in tetrahydrofuran/acetonitrile/methanol (15:30:55, v/v/v), injection on a $C_{18}$ column with methanol/acetonitrile (90:10, v/v) + triethylamine $9{\mu}M$ as mobile phase, and ${\lambda}_{detection}$=475 nm. The mean percent recovery for the HPLC method were $120.7{\pm}4.1%$ (lycopene), $89.2{\pm}3.5%$ (lutein), $91.2{\pm}2.9%$ (${\alpha}$-carotene), $99.1{\pm}4.4%$ (${\beta}$-carotene), and $100.0{\pm}5.3%$ (cryptoxanthin). The contents of lutein in the agricultural products were spinach, kiwi, tomato, blueberry, melon, respectively. However, the lycopene contents were the highest in the Black tomato ($56.66{\pm}7.48mg/kg$) and Jangseong tomato ($50.28{\pm}5.42mg/kg$). The concentration of ${\beta}$-carotene in all of the agricultural products ranged from 0.07 mg/kg to 65.03 mg/kg. The quercetin content of the agricultural products increased in the order of blueberry (986.57~1,054.06 mg/100 g), kiwi (44.96~55.09 mg/100 g), hallabong (31.92~35.60 mg/100 g), and tomato (26.38~34.94 mg/100 g). The highest kaempferol content was found in the blueberry (47.79~76.15 mg/100 g) with results in all of the tested samples varying between 6.54~48.11 mg/100 g. The total polyphenol contents of the various agricultural products increased in the blueberry (213.60~229.96 mg/100 g), spinach (112.50~141.67 mg/100 g) and kiwi (46.49~70.44 mg/100 g). The total flavonoid content was the highest in both blueberry and spinach. Vitamin C content was detected in kiwi > hallabong > tomato > blueberry, respectively. The total anthocyanin contents (TAC) was detected in the Damyang blueberry and the imported blueberry.
Oldenlandia diffusa is a Chinese medicinal herb with antitumor activity capable of suppressing the growth of some cancer cell lines. Oleanolic acid and ursolic acid are triterpenoid compounds that exist in Oldenlandia diffusa. Recently, these have been noted for anti-inflammatory, anti-cancer, and hepato-protective effects. Application of both plant growth regulators, 2,4-D and kinetin, was found to be essential for the initiation of callus and suspension cells. Leaf blades of Oldenlandia diffusa was transformed into callus on Schenk and Hildebrandt medium supplemented with 0.5 mg/L 2,4-D and 0.1 mg/L kinetin, while optimum initiation condition for suspension cells of Oldenlandia diffusa was determined to be 0.75 mg/L 2,4-D and 0.1 mg/L kinetin. Chromatographic separation of oleanolic acid from its derivatives was achieved using Rexchrom S5-100-ODS column. Analytical conditions for oleanolic acid were determined as follows: flow rate at 1.0 mL/min, UV length at 200 nm and mobile phase of $80\%$ acetonitrile and $20\%$ water. Production of secondary metabolites was found to be increased by the treatment with elicitors or signal transducers. The maximum production of oleanolic acid was 99.6 mg/L in cultures with 0.5 mM salicylic acid. It is 1.74 times higher than that of control.
Kang, Dong Hyeon;Han, Eun Hye;Jin, Changbae;Kim, Hyoung Ja
Journal of the Korean Society of Food Science and Nutrition
/
v.45
no.11
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pp.1610-1616
/
2016
This study aimed to establish an optimal extraction process and high performance liquid chromatography-ultraviolet (HPLC-UV) analytical method for determination of 3,5-dicaffeoylquinic acid (3,5-DCQA) as a part of materials standardization for the development of a xanthine oxidase inhibitor as a health functional food. The quantitative determination method of 3,5-DCQA as a marker compound was optimized by HPLC analysis using a Luna RP-18 column, and the correlation coefficient for the calibration curve showed good linearity of more than 0.9999 using a gradient eluent of water (1% acetic acid) and methanol as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 320 nm. The HPLC-UV method was applied successfully to quantification of the marker compound (3,5-DCQA) in Aster glehni extracts after validation of the method with linearity, accuracy, and precision. Ethanolic extracts of A. glehni (AGEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 30, 50, 70, and 80% ethanol for 3, 4, 5, and 6 h, respectively. Among AGEs, 70% AGE at $70^{\circ}C$ showed the highest content of 3,5-DCQA of $52.59{\pm}3.45mg/100g$ A. glehni. Furthermore, AGEs were analyzed for their inhibitory activities on uric acid production by the xanthine/xanthine oxidase system. The 70% AGE at $70^{\circ}C$ showed the most potent inhibitory activity with $IC_{50}$ values of $77.01{\pm}3.13{\sim}89.96{\pm}3.08{\mu}g/mL$. The results suggest that standardization of 3,5-DCQA in AGEs using HPLC-UV analysis would be an acceptable method for the development of health functional foods.
Journal of the Korea Institute of Information and Communication Engineering
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v.4
no.1
/
pp.77-88
/
2000
In this paper, the 3-mode variable gain high power amplifier for a transmitter of INMARSAT-B operating at L-band(1626.5-1646.5 MHz) was developed. This SSPA can amplify 42 dBm in high power mode, 38 dBm in medium power mode and 36 dBm in low power mode for INMARSAT-B. The allowable errol sets +1 dBm as the upper limit and -2 dBm as the lower limit, respectively. To simplify the fabrication process, the whole system is designed by two parts composed of a driving amplifier and a high power amplifier. The HP's MGA-64135 and Motorola's MRF-6401 were used for driving amplifier, and the ERICSSON's PTE-10114 and PTF-10021 for the high power amplifier. The SSPA was fabricated by the RP circuits, the temperature compensation circuits and 3-mode variable gain control circuits and 20 dB parallel coupled-line directional coupler in aluminum housing. In addition, the gain control method was proposed by digital attenuator for 3-mode amplifier. Then il has been experimentally verified that the gain is controlled for single tone signal as well as two tone signals. In this case, the SSPA detects the output power by 20 dB parallel coupled-line directional coupler and phase non-splitter amplifier. The realized SSPA has 41.6 dB, 37.6 dB and 33.2 dB for small signal gain within 20 MHz bandwidth, and the VSWR of input and output port is less than 1.3:1. The minimum value of the 1 dB compression point gets more than 12 dBm for 3-mode variable gain high power amplifier. A typical two tone intermodulation point has 36.5 dBc maximum which is single carrier backed off 3 dB from 1 dB compression point. The maximum output power of 43 dBm was achieved at the 1636.5 MHz. These results reveal a high power of 20 Watt, which was the design target.
Preferential flow has recently been the subject of increasing interest because these phenomena contribute to solute transport in soils. Commonly, preferential flow paths are associated with macropores or highly structured soils. We presented an analysis of the measured breakthrough curves (BTCs) of $Cl^-$ and $Cu^{2+}$ ions to test the occurrence of preferential flow in soils using miscible displacement technique under steady flow conditions. We also analyzed soil water retention curves and from this curves induced cumulative pore size distribution of undisturbed soils, which sampled from Ap1, B1, and C horizons of Songjeong series soils (the fine loamy, mesic family of Typic Hapludults). In this study, miscible displacement experiment on C horizon was excluded, because it is structureless sandy loam with saturated hydraulic conductivity of $5.2cmhr^{-1}$. The saturated hydraulic conductivity of Ap1 horizon was $2.0cmhr^{-1}$, which was about 7 times higher than that of B1 horizon ($0.27cm hr^{-1}$). Cumulative pore size distribution predicted that Ap1 horizon had more macropores (pore diameter larger than $49{\mu}m$, equivalent to -6 kpa of soil matric potential) than B1 horizon. The hydrodynamic dispersion coefficient from chloride BTCs was estimated as $1.3cm^2hr^{-1}$ for B1 and $34cm^2hr^{-1}$ for Ap1 horizon. However the retardation factors of B1 and Ap1 horizon were significantly different, i.e. 1 and 0.6, respectively, which means that there was distinct partition between mobile water and immobile phase in Ap1 horizon. The copper retardation effect of Ap1 horizon was less than that of B1 horizon, even though cation exchange capacity of Ap1 horizon was higher than that of B1 horizon. Thus, breakthrough curves of $Cl^-$ and $Cu^{2+}$ obviously showed the probability that preferential flow would occur in Ap1 horizon.
Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.
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