• Journal of Food Hygiene and Safety
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• v.34 no.6
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• pp.519-525
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• 2019

The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we are continuing our research on analytical method development for the items listed in the Korean Health Functional Food Codex. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determine coenzyme Q10 based on liquid chromatographic-tandem mass spectrometry (LC-MS/MS). Calibration curves showed linearity with a correlation coefficient (R²) of > 0.999 and the limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 26.0 ㎍/L and 78.9 ㎍/L, respectively. The recovery results ranged between 98.6-107.0% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high resolution of the coenzyme Q10 and the assay was fully validated as well.

• Journal of Korean Society of Water and Wastewater
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• v.28 no.2
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• pp.207-215
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• 2014

Wastewater containing heavy metals such as copper (Cu) and nickel (Ni) is harmful to humans and the environment due to its high toxicity. Crystallization in a fluidized bed reactor (FBR) has recently received significant attention for heavy metal removal and recovery. It is necessary to find optimum reaction conditions to enhance crystallization efficacy. In this study, the effects of crystallization reagent and pH were investigated to maximize crystallization efficacy of Cu-S and Ni-S in a FBR. CaS and $Na_2S{\cdot}9H_2O$ were used as crystallization reagent, and pH were varied in the range of 1 to 7. Additionally, each optimum crystallization condition for Cu and Ni were sequentially employed in two FBRs for their selective removal from the mixture of Cu and Ni. As major results, the crystallization of Cu was most effective in the range of pH 1-2 for both CaS and $Na_2S{\cdot}9H_2O$ reagents. At pH 1, Cu was completely removed within five minutes. Ni showed a superior reactivity with S in $Na_2S{\cdot}9H_2O$ compared to that in CaS at pH 7. When applying each optimum crystallization condition sequentially, only Cu was firstly crystallized at pH 1 with CaS, and then, in the second FBR, the residual Ni was completely removed at pH 7 with $Na_2S{\cdot}9H_2O$. Each crystal recovered from two different FBRs was mainly composed of CuxSy and NiS, respectively. Our results revealed that Cu and Ni can be selectively recovered as reusable resources from the mixture by controlling pH and choosing crystallization reagent accordingly.

• Journal of Pharmaceutical Investigation
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• v.35 no.3
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• pp.137-142
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• v.35 no.6
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• pp.437-443
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• v.35 no.4
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• pp.265-271
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• v.35 no.6
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• pp.423-429
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• 2005

A selective and sensitive reversed-phase HPLC method for the determination of fenoprofen in human serum was developed, validated, and applied to the pharmacokinetic study of fenoprofen calcium. Fenoprofen and internal standard, ketoprofen, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Luna C18(2) column with the mobile phase of acetonitrile-3 mM potassium dihydrogen phosphate (32:68, v/v, adjusted to pH 6.6 with phosphoric acid). Detection wavelength of 272 nm and flow rate of 0.25 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fenoprofen concentration $(2\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-100\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was $0.05\;{\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.27 to 109.20% for fenoprofen with overall precision (% C.V.) being 5.51-11.71 %. The relative mean recovery of fenoprofen for human serum was 81.7%. Stability (freeze-thaw, short and long-term) studies showed that fenoprofen was not stable during storage. But, extracted serum sample and stock solution were allowed to stand at ambient temperature for 12 hr prior to injection without affecting the quantification. The peak area and retention time of fenoprofen were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fenoprofen in human serum samples for the pharmacokinetic studies of orally administered Fenopron tablet (600 mg as fenoprofen) at three different laboratories, demonstrating the suitability of the method.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.7 no.1
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• pp.25-31
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• 2009

An analytical method of $^{99}Tc$ concentration in soil was set up and discussed considering the $^{99}Tc$ concentration in Korean soil measured with its analytical method. A selective TEVA resin was used to separate and purify the $^{99}Tc$ in the soil sample. $^{99m}Tc$ from a commercial $^{99}Mo/^{99m}Tc$ generator was used as a yield tracer for the chemical separation of $^{99}Tc$ and its problem when using $^{99m}Tc$ as a tracer was discussed. The chemical recovery yield of $^{99}Tc$ was above 70%. The optimum conditions of inductively coupled plasma mass spectrometry system(ICP-MS) were set up to determine the $^{99}Tc$ after the separation process. The minimum detectable activity(MDA) was 15 mBq/kg-dry in this analytical procedure. The $^{99}Tc$ concentration in soils of Jeju and Kori were measured in the rage of 33.73-89.16 mBq/kg-dry. Those values were less than those reported in other countries and seemed to be originated from atmospheric fallout.

• Journal of Pharmaceutical Investigation
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• v.36 no.2
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• pp.89-95
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• 2006

A selective and sensitive reversed-phase HPLC method for the determination of pentoxifylline in human serum was developed, validated, and applied to the pharmacokinetic study of pentoxifylline. Pentoxifylline and internal standard, chloramphenicol, were extracted from the serum by liquid-liquid extraction with dichloromethane and analyzed on a Luna CI8(2) column with the mobile phase of acetonitrile-0.034 M phosphoric acid (25:75, v/v, adjusted to pH 4.0 with 10 M NaOH). Detection wavelength of 273 nm and flow rate of 0.8 mL/min were used. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of the serum was 10 ng/mL, which was sensitive enough for pharmacokinetic studies of pentoxifylline. The overall accuracy of the quality control samples ranged from 89.3 to 92.7% for pentoxifylline with overall precision (% C.V.) being 4.1-9.2%. The relative mean recovery of pentoxifylline for human serum was 105.8%. Stability (stock solution, short and long-term) studies showed that pentoxifylline was not stable during storage. But three freeze-thaw cycles and extracted serum samples were stable. This method showed good ruggedness (within 15% C.V.) and was successfully applied for the analysis of pentoxifylline in human serum samples for the pharmacokinetic studies of orally administered $Trental^{\circledR}$ tablet (400 mg pentoxifylline), demonstrating the suitability of the method.

• Resources Recycling
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• v.24 no.3
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• pp.44-50
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• 2015

Recycling technologies would be required in consideration of increasing demand in lithium ion batteries (LIBs). In this study, the leaching behavior of Ni, Co and Mn is investigated with ammoniacal medium for spent cathode active materials, which are separated from a commercial LIB pack in hybrid electric vehicles. The leaching behavior of each metal is analyzed in the presence of reducing agent and pH buffering agent. The existence of reducing agent is necessary to increase the leaching efficiency of Ni and Co. The leaching of Mn is insignificant even with the existence of reducing agent in contrast to Ni and Co. The most conspicuous difference between acid and ammoniacal leaching would be the selective leaching behavior between Ni/Co and Mn. The ammoniacal leaching can reduce the cost of basic reagent that makes the pH of leachate higher for the precipitation of leached metals in the acid leaching.

• Resources Recycling
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• v.20 no.6
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• pp.50-55
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• 2011

Using ultrasonic irradiation, the separation and recovery of PV cell, made of silicon wafer, from PV module was carried out through selective decomposition of EVA used as an interlaminated binder. The ultrasonic cleaner of bath-type (Output: 130 W, Frequency: 40 kHz) was used as an ultrasonic apparatus in this research. With the fixed distance of 2 cm, from ultrasonic generator to PV cell, the experiment of EVA decomposition was performed in various organic solvents such as Toluene, Trichloroethylene, O-dichlorobenzene, Benzene. And also their concentrations and temperature was changed to survey the optimum conditions. However EVA can be decomposed perfectly at $55^{\circ}C$ within 160 min in 5 M of all kinds of solvent, PV cell may be recovered with being damaged or broken severely. This damage may be resulted from the swelling of EVA in the process of decomposition. Whereas, at the condition of 5 M at $65^{\circ}C$, PV cell can be recovered with the state of minor damage or crack. This implies that the decomposition rate of EVA increases with an increase of temperature, thereby EVA can be decomposed before the swelling of EVA layer. Conclusively, it is possible for PV cell to be recovered within 40 min, at $65^{\circ}C$ in 5 M, with less damage.