• Korean Journal of Pharmacognosy
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• v.50 no.1
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• pp.65-71
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• 2019

One of the oriental medicine prescriptions, Sagunja-tang consists of four herbal medicines (Ginseng Radix, Poria Sclerotium, Atractylodis Rhizoma Alba, and Glycyrrhiziae Radix et Rhizoma) and has been used as a medicine to enhance tonify the function of spleen and stomach in Korea. In this study, we conducted simultaneous analysis of the 9 marker components, liquiritin apioside, liquiritin, ginsenoside Rg1, liquiritigenin, ginsenoside Rb1, glycyrrhizin, atractylenolide III, atractylenolide II, and atractylenolide I in Sagunja-tang using a liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Marker compounds were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, 1.7 mm) and the column was maintained at $45^{\circ}C$. The mobile phase consists of 0.1% (v/v) aqueous formic acid and acetonitrile with gradient condition. The LC-MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS system with multiple reaction monitoring (MRM) method in the positive and negative modes. The calibration curves of the nine marker components showed good linearity with coefficient of determination ${\geq}0.9984$ within tested range. The limits of detection and limits of quantification values were 0.27-2.42 ng/mL and 0.81-7.27 ng/mL, respectively. The concentrations of tested 9 analytes in the lyophilized Sagunja-tang sample using the established LC-ESI-MS/MS MRM method were detected up to 16.593 mg/g. These results can be useful as a basic data for the quality control of an oriental medicine prescriptions.

• Biomolecules & Therapeutics
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• v.27 no.2
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• pp.193-200
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• 2019

Ceramide metabolism is known to be an essential etiology for various diseases, such as atopic dermatitis and Gaucher disease. Glucosylceramide synthase (GCS) is a key enzyme for the synthesis of glucosylceramide (GlcCer), which is a main ceramide metabolism pathway in mammalian cells. In this article, we developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine GCS activity using synthetic non-natural sphingolipid C8-ceramide as a substrate. The reaction products, C8-GlcCer for GCS, could be separated on a C18 column by reverse-phase high-performance liquid chromatography (HPLC). Quantification was conducted using the multiple reaction monitoring (MRM) mode to monitor the precursor-to-product ion transitions of m/z $588.6{\rightarrow}264.4$ for C8-GlcCer at positive ionization mode. The calibration curve was established over the range of 0.625-160 ng/mL, and the correlation coefficient was larger than 0.999. This method was successfully applied to detect GCS in the human hepatocellular carcinoma cell line (HepG2 cells) and mouse peripheral blood mononuclear cells. We also evaluated the inhibition degree of a known GCS inhibitor 1-phenyl-2-decanoylamino-3-morpholino-1-propanol (PDMP) on GCS enzymatic activity and proved that this method could be successfully applied to GCS inhibitor screening of preventive and therapeutic drugs for ceramide metabolism diseases, such as atopic dermatitis and Gaucher disease.

• Mass Spectrometry Letters
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• v.12 no.1
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• pp.1-10
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• 2021

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

• Progress in Medical Physics
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• v.9 no.3
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• pp.137-141
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• 1998

The purposes of this report are to evaluate whether lead ball and steel ball could be used as protective material of radiation and to acquire physical data of them for protecting 4-10 MV X-ray beams. Lead balls of diameter 2.0～2.5mm or steel balls of diameter 1.5～2.0 mm were filled in an acrylic box of uniform width. An MV radiograph of metal balls in a box were taken to ascertain uniformity of ball distribution in the box. Average density of metal ball and linear attenuation coefficient of metal balls for 4～10 MV X -rays were measured. At the time of measurement of linear attenuation coefficient, Farmer ionization chamber was used and to minimize the scatter effect, distance between the ball and the ionization chamber was 70 cm and field size was 5.5cm${\times}$5.5cm. For comparison, same parameters of lead and steel plates were measured. The distribution of metal balls was uniform in the box. The density of a mixture of lead-air was 6.93g/cm$^3$, 0.611 times density of lead, and the density of a mixture of steel-air was 4.75g/cm$^3$, 0.604 times density of steel. Half-value layers of a mixture of lead-air were 1.89 cm for 4 MV X-ray, 2.07 cm for 6 MV X-ray and 2.16 cm for 10 MV X-ray, and approximately 1.64 times of HVL of lead plate. Half-value layers of a mixture of steel-air were 3.24 cm for 4 MV X-ray, 3.70 cm for 6 MV X-ray and 4.15 cm for 10 MV X-ray, and approximately 1.65 times of HVL of lead plate. Metal balls can be used because they could be distributed evenly. Average densities of mixtures of lead-air and steel-air were 6.93g/cm$^3$, 4.75g/cm$^3$ respectively and approximately 1.65 times of densities of lead and steel. Product of density and HVL for a mixture of metal-air are same as the metal.

• Progress in Medical Physics
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• v.20 no.2
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• pp.97-105
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• 2009

Absorbed dose to water based protocols recommended that plane-parallel chambers be calibrated against calibrated cylindrical chambers in a high energy electron beam with $R_{50}$>7 $g/cm^2$ (E${\gtrsim}$16 MeV). However, such high-energy electron beams are not available at all radiotherapy centers. In this study, we are compared the absorbed dose to water determined according to cross-calibration method in a high energy electron beam of 16 MeV and in electron beam energies of 12 MeV below the cross-calibration quality remark. Absorbed dose were performed for PTW 30013, Wellhofer FC65G Farmer type cylindrical chamber and for PTW 34001, Wellhofer PPC40 Roos type plane-parallel chamber. The cylindrical and the plane-parallel chamber to be calibrated are compared by alternately positioning each at reference depth, $Z_{ret}=0.6R_{50}-0.1$ in water phantom. The $D_W$ of plane-parallel chamber are derived using across-calibration method at high-energy electron beams of 16, 20 MeV. Then a good agreement is obtained the $D_W$ of plane-parallel chamber in 12 MeV. The agreement between 20 MeV and 12 MeV are within 0.2% for IAEA TRS-398.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.45 no.1
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• pp.69-75
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• 2019

Preservatives of cosmetics is managed by positive list in Korea. Positive list requires a proper quantitative analysis method, but the analysis method is still insufficient. In this study, gas chromatography with flame ionization detector was used to simultaneously analyze 14 preservatives in cosmetics. As a result of method validation, the specificity was confirmed by the calibration curves of 14 preservatives showing good linearity correlation coefficient of above 0.9997 except dehydroacetic acid (0.9891). The limits of detection (LOD) and quantification (LOQ) of 14 preservatives were 0.0001 mg/mL ~ 0.0039 mg/mL and 0.0003 mg/mL ~ 0.0118 mg/mL, respectively, but they were 0.0204 mg/mL, 0.0617 mg/mL for dehydroacetic acid, respectively. The precision (Repeatability) of the values was less than 1.0%, but 7.1% for dehydroacetic acid. The Accuracy (% recovery) of 14 preservatives in cosmetics showed 96.9% ~ 109.2%. Finally, this method was applied to 50 cosmetics available in market. Results showed that the commonly used preservatives were chlorophene, phenoxyethanol, benzyl alcohol and parabens. However, the amount of the detected preservatives was within maximum allowed limits established by KFDA.

• Korean Journal of Environmental Agriculture
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• v.35 no.3
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• pp.166-174
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• 2016

BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C₁₈ column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R²≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

• Analytical Science and Technology
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• v.26 no.2
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• pp.154-163
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• 2013

The maximum residue limits of pyrimisulfan is set as 0.05 mg/kg in rice in 2011, so very reliable and sensitive analytical method for pyrimisulfan residues is required for ensuring the food safety of pyrimisulfan residues in agricultural products. In this study, a rapid and sensitive analytical method was developed and validated using liquid chromatography electrospray ionization tandem mass spectrometry (LC-MS/MS) for the determination of herbicide pyrimisulfan residues in agricultural products. Average recoveries of pyrimisulfan ranged from 88.7 to 99.3% at the spiked level of 0.005 mg/kg and from 90.1 to 94.2% at the spiked level of 0.05 mg/kg, while the relative standard deviation was less than 10%. Linear range of pyrimisulfan was between 0.01~1.0 ${\mu}g/mL$ with the correlation coefficient ($r^2$) 0.999 and limit of quantification was 0.005 mg/kg. The results of method validation were satisfied Codex guideline. The results revealed that the developed and validated analytical method is possible for pyrimisulfan determination in agricultural product samples and will be used as an official analytical method.

• Journal of Ginseng Research
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• v.37 no.1
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• pp.135-141
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• 2013

A rapid, sensitive and selective analytical method was developed and validated for the determination of compound K, a major intestinal bacterial metabolite of ginsenosides in human plasma. Liquid-liquid extraction was used for sample preparation and analysis, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Compound K was analyzed on a Phenomenex Luna C18 column ($100{\times}2.00$ mm, 3 ${\mu}m$) with the mobile phase run isocratically with 10 mM ammonium acetate-methanol-acetonitrile (5:47.5:47.5, v/v/v) at a flow rate of 0.5 mL/min. The method was validated for accuracy (relative error <12.63%), precision (coefficient of variation <9.14%), linearity, and recovery. The assay was linear over the entire range of calibration standards i.e., a concentration range of 1 ng/mL to 1,000 ng/mL ($r^2$ >0.9968). The recoveries of compound K after liquid-liquid extraction at 1, 2, 400, and 800 ng/mL were $106.00{\pm}0.08%$, $103.50{\pm}0.19%$, $111.45{\pm}5.21%$, and $89.62{\pm}34.46%$ for intra-day and $85.40{\pm}0.08%$, $94.50{\pm}0.09%$, $112.50{\pm}5.21%$, and $95.87{\pm}34.46%$ for inter-day, respectively. The lower limit of quantification of the analytical method of compound K was 1 ng/mL in human plasma. The developed method was successfully applied to a pharmacokinetic study of compound K after oral administration in ten of healthy human subjects.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.1
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• pp.37-44
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• 2014

Preservatives such as paraben, phenoxyethanol, and chlorphene are commonly used in cosmetics thanks to cheap price and good antiseptic effect. Recently, consumers' concerns about their possible toxicity and skin irritation forced them to be replaced with straight 1,2-alkanediols. However, as the alkanediols may also irritate skin, limited amount of them should be used in cosmetics. Three 1,2-alkanediols including 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol in cosmetics were analyzed simultaneously by gas chromatogrphy with flame ionization detector. As a result of method validation, the specificity was confirmed by the calibration curves of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol showing good linearity correlation coefficient of above 0.999 over the concentration range of $100{\sim}1,200{\mu}g/g$. The limit of detection (LOD) and quantification (LOQ) of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol were 31, 40, and $19{\mu}g/g$ and 98, 108, and $57{\mu}g/g$, respectively. The precision (Repeatability) of the amount in cosmetics showed less than 2.0%. Relative Standard Deviation (% RSD) and the Accuracy (% recovery) of the amount in cosmetics showed 99.3 ~ 103.3, 99.4 ~ 106.7, 97.5 ~ 107.3% respectively. As a result, simultaneous analysis of antimicrobial three 1,2-alkanediols in cosmetics were possible. This method can be utilized in accurate quantitative analysis of 1,2-alkanediols in cosmetics.