• Analytical Science and Technology
• /
• v.32 no.2
• /
• pp.35-47
• /
• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• Analytical Science and Technology
• /
• v.33 no.6
• /
• pp.233-239
• /
• 2020

This study was performed to develop an analytical method using Carrez reagents as the precipitant to effectively and easily remove proteins and lipids while pretreating samples for the simultaneous determination of preservatives, including dehydroacetic acid (DHA), sorbic acid (SA), benzoic acid (BA), methyl ρ-hydroxybenzoate (MP), ethyl ρ-hydroxybenzoate (EP), propyl ρ-hydroxybenzoate (PP), isopropyl ρ-hydroxybenzoate (IPP), butyl ρ-hydroxybenzoate (BP), and isobutyl ρ-hydroxybenzoate (IBP). The effective selectivity was determined by HPLC separation analysis for nine preservatives in the test solution, after removing interfering materials such as lipids and proteins. The method developed in this study showed excellent linearity at 0.999 or higher. The limit of detection (LOD) ranged from 0.09 to ~0.12 mg/L and the limit of quantitation (LOQ) was ~0.280.37 mg/L. The results of the recovery test on processed foods, including pickles, cheeses, processed meat products, beverages, sauces, and emulsified foods showed DHA, SA, BA, MP, EP, IPP, PP, IBP, and BP at 90.9~107.7 %, 85.4~113.7 %, 90.7~111.6 %, 84.5~111.2 %, 81.3~110.9 %, 82.5~102.2 %, 81.1~110.0 %, 80.9~109.0 %, and 82.4~110.3 %, respectively. The probability of the simultaneous analytical method developed in this study as a quantitative method was confirmed for various processed foods.

• Membrane Journal
• /
• v.31 no.3
• /
• pp.228-240
• /
• 2021

The organic solvent robust polybenzimidazole (PBI) membranes were prepared as organic solvent nanofiltration (OSN) membrane for the recycling of alcoholic solvents using non-solvent induced phase separation with different dope solution concentration and coagulant composition of water/ethanol mixtures to control the membrane morphology and permeation performance. Investigation on crosslinking of polybenzimidazole indicated that the membrane crosslinked with dibromoxylene (DBX) had enough mechanical strength and solvent resistance to be applied as a OSN membranes. The crosslinked PBI membrane prepared by more than 20wt% dope concentration coagulated in water showed a rejection of > 90% to Congo Red (MW of 696.66 g/mol) while pure ethanol permeances was more than 22.5 LMH/bar at 5 bar. Investigation on coagulant composition indicated that ethanol permeance through crosslinked PBI OSN membrane increased with increasing of ethanol concentration in water/ethanol mixture coagulants.

• Analytical Science and Technology
• /
• v.35 no.6
• /
• pp.256-266
• /
• 2022

It is important to determine the concentration of long-lived radionuclides (e.g., ¹²⁹I) in nuclear waste to ensure safety when handling it. To analyze nuclides in a solid sample (e.g., concrete and soil), it is essential to effectively separate and purify the nuclides of interest in the sample. This study reports the comprehensive efforts made to validate the analytical procedure for ¹²⁹I detection in solid samples, using a high-temperature combustion furnace. ¹²⁹I volatilized from the sample collected in 0.01 M HNO₃ solution with a reducing agent (e.g., NaHSO₃) and was rapidly measured by ICP-MS. Analytical conditions, such as pyrolysis temperature and types of mobile phase gas, catalyst, and trapping solution, were optimized to obtain a high recovery rate of spiked ¹²⁹I. Finally, the optimized method was applied for the simultaneous analysis of other volatile radionuclides, such as ³H and ¹⁴C. The performance test results for the optimized method confirmed that the LSC (for ³H and ¹⁴C) and ICP-MS (for ¹²⁹I) measurements, with the separation of volatile nuclides using a high-temperature combustion furnace, were reliable.

• Korean Journal of Environmental Agriculture
• /
• v.42 no.3
• /
• pp.203-210
• /
• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Journal of the Korean Recycled Construction Resources Institute
• /
• v.11 no.1
• /
• pp.55-61
• /
• 2023

This study aims to develop CLSM fill material for emergency restoration using landfill coal ash. As a result of examining physical properties such as particle size distribution and fines content of landfill coal ash, bottom ash, fly ash, and general soil were mixed, and SP was found to have a density of 2.03 and a residual particle pass rate of 7.8 %. CLSM materials that secure fluidity in unit quantities without using chemical admixtures such as glidants and water reducing agents have a high risk of material separation due to bleeding. As a result of this experiment, it was found that the bleeding ratio did not satisfy the standard in the case of the specimen with a large amount of fly ash and a lot of addition of mixing water. As a result of the compressive strength test, the strength development of 0.5 MPa or more for 4 hours was found to be satisfactory for the specimens using hemihydrate gypsum with a unit binder amount of 200 or more, and the remaining gypsum showed poor strength development. Although it is judged that landfill coal ash can be used as a CLSM material, it is necessary to identify and apply the physical and chemical characteristics of coal ash buried in the ash treatment plant of each power generation company.

• Resources Recycling
• /
• v.32 no.2
• /
• pp.3-11
• /
• 2023

The aim of this study was to develop a physical treatment method for obtaining iron concentrate with a grade higher than 60% from slag generated in the Waelz Kiln (WK) process. The size of the WK slag used in this work was several millimeters, with T-Fe and ZnO contents of 40.24% and 1.03%, respectively. The slag samples were pulverized in a laboratory rod mill for various grinding times, followed by a magnetic separation test under a low magnetic intensity of 0.05 T initially. The results showed that the highest iron grade was obtained from samples with a grinding time of 10 min. Additionally, for a grinding time of 20 min, the highest grade and recovery ratios were achieved at a magnetic intensity of 0.8 T. Based on these findings, the optimal physical treatment process proposed in this study resulted in iron concentrates with a grade of 61.34% and an enrichment ratio of 1.52.

• Analytical Science and Technology
• /
• v.20 no.4
• /
• pp.347-354
• /
• 2007

A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

• The Journal of the Convergence on Culture Technology
• /
• v.9 no.6
• /
• pp.867-873
• /
• 2023

In this study, for the purpose of standardized quality control of a cold medicine, we simultaneous analyzed four main chemical components of a cold medicine: acetaminophen, caffeine, methyl paraben, and propyl paraben. The sample was subjected to quantitative analysis using high performance liquid chromatography (HPLC), after pretreatment of four components. The experiment was carried out by using Isocratic elution at wavelength of 270nm. Acetonitrile and water (H₂O) were used as a mobile phase at a flow rate of 1.0mL/min in a commercial C18 reversed-phase column. A volume of 10uL cold medicine were injected into the column with column oven temperature at 35℃. As a result of the experiment, the values of Resolution were 4.983, 1.596, 5.519, and 1.678 respectively-well over Rs >1.5, which indicates that the separation of four components were efficient. In addition, value of symmetry factor of the components was 1.056, 1.069, 1.032, and 1.133 respectively, to show its symmetrical stability. The calibration curve of all four components exhibits good linearity with R² >0.9995 to 0.9999. Furthermore, the limit of detection(LOD) were between 0.0118 to 1.5973 mg/mL, while the limit of quantification (LOQ) were between 0.0353 to 4.7919 ㎍/mL with the recovery rate of 79.6% ~ 120.5%. The results of this study showed an efficient quality evaluation of a simultaneous analysis method for cold medicine components.

• Sim-seong Yeon-gu
• /
• v.31 no.2
• /
• pp.177-214
• /
• 2016

This thesis is an interpretation of "Golden bird" of Grimm's fairy tale and similar other tales from the perspective of analytical psychology. Golden bird story start loss of golden apple in king's garden. King and three sons are one-sided structure live without female members in family. They need feminine aspect. Adventure and journey of stupid youngest son can be seen as a individuation process in analytic psychology. Ego meets several painful experience during journey. New Kingdom has a new specific collective consciousness. When ego fixed dominated specific collective consciousness he can only be liberated after completing the difficult task of the next phase in crisis of death. This process is initiation, which is a supplement to feminity after recovery of increased consciousness, marriage with the princess, which is possible to unify the sexes (coniunctio oppositorum). The ego who got the apple, bird, horse, and princess which is shown to be a supplement to feminity, does not attain a complete success. Although the youngest comes out after brothers' failure, yet separation and abandonment of persona are difficult challenges and after all he achives a higher consciousness and then he primarily marries the princess, his Anima, after he executed his brothers for his repeated hardships, when the intellectual capacity is sacrificed as offering. Also, the fox restores himself from magic after the youngest son kills him and cut his head and feet, as the fox's wish. To be transformed into a human being. It experiences another consciousness. Finally, unifying the coniunctio oppositerum is fulfilled and a divine bond achieves the wholeness and it is accomplished individuation. In clinical practice, fox is compared to a therapist as a guide of individuation process who lead clients.