• Korean Journal of Veterinary Service
• /
• v.42 no.4
• /
• pp.289-296
• /
• 2019

A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C₁₈ sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R²) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.

• The Korea Journal of Herbology
• /
• v.26 no.1
• /
• pp.41-46
• /
• 2011

Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.

• Journal of Pharmaceutical Investigation
• /
• v.40 no.2
• /
• pp.101-107
• /
• 2010

A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of N-(-4-Chlorophenyl)-6-hydroxy-7-methoxy-2-chromanecarboxamide (KAL-1120), a novel anti-inflammation agent, in the rat plasma. The method was applied to analyze the compound in the biological fluids such as bile, urine and tissue homogenates. After liquid-liquid extraction, the compound was analyzed on an HPLC system with ultraviolet detection at 275 nm. HPLC was carried out using reversed-phase isocratic elution with a $C_{18}$ column, a mobile phase of a mixture of acetonitril (40 v/v%) at a flow rate of 1.0 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma was linear over the concentration range of 0.05-50 ${\mu}g$/mL. The intra- and inter-day assay accuracies of this method ranged from 0.06% to 9.33% of normal values and the precision did not exceed 6.28% of relative standard deviation. The plasma concentration of KAL-1120 decreased to below the quantifiable limit at 1.5 hr after the i.v. bolus administration of 2-10 mg/kg to rats ($t_{1/2,({\alpha})}$ and $t_{1/2,({\beta})$ of 2.15 and 26.7 min at a dose of 2 mg/kg, 3.91 and 33.0 min at a dose of 10 mg/kg, respectively). The steady-state volume of distribution ($V_{dss}$) and the total body clearance ($CL_t$) were not significantly altered in rats given doses from 2 to 10 mg/kg. Of the various tissues tested, KAL-1120 was mainly distributed in the lung and heart after i.v. bolus administration. KAL-1120 was detected in the bile by 30 min after its i.v. bolus administration. However, the concentration in the urine after i.v. bolus administration became too low to measure, suggesting that KAL-1120 is mostly excreted in the bile. In conclusion, this analytical method was suitable for the preclinical pharmacokinetic studies of KAL-1120 in rats.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.44 no.11
• /
• pp.1682-1686
• /
• 2015

This study was conducted to establish an HPLC analysis method for determination of marker compounds as part of materials standardization for development of health functional food materials from pear pomace. The quantitative determination method of caffeic acid and chlorogenic acid as marker compounds of pear pomace extract (PPE) was optimized by HPLC analysis using a C18 column ($5{\times}250mm$, $5{\mu}m$) with a 0.2% elution gradient of acetic acid and methanol as the mobile phase at a flow rate of 0.8 mL/min and detection wavelength of 330 nm. The HPLC/UV method was applied successfully to the quantification of marker compounds in PPE after validation of the method with linearity, accuracy, and precision. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999, and limit of detection and limit of quantification were $1.14{\mu}g/mL$ (caffeic acid) and $1.61{\mu}g/mL$ (chlorogenic acid) as well as $4.9{\mu}g/mL$ (caffeic acid) and $4.9{\mu}g/mL$ (chlorogenic acid), respectively. Relative standard deviation values from intra- and inter-day precision were less than 3.1% (caffeic acid) and 4.0% (chlorogenic acid), respectively. Recovery rates of caffeic acid and chlorogenic acid at 12.5, 25, and $50{\mu}g/mL$ were 93.66~106.32% and 97.33~105.68%, respectively. An optimized method for extraction of caffeic acid and chlorogenic acid in PPE was established through diverse extraction conditions, and the validation indicated that the method is very useful for evaluation of marker compounds in PPE to develop a health functional food material.

• Food Science and Preservation
• /
• v.24 no.6
• /
• pp.795-801
• /
• 2017

Aralia elata Seemann (AE) has long been used as a folk medicine for the treatment of various diseases including diabetes mellitus, anti-arthritic, and anti-gastric ulcer agent in Korea, Japan, and China. This study was performed to establish a simple and reliable HPLC/UV analytical method for determination of most active anti-hypertensive compound, a 3-O-${\alpha}$-L-rhamnopyranosyl($1{\rightarrow}$2)-${\alpha}$-L-arabinopyranosyl hederagenin 28-O-${\beta}$-D-xylopyranosyl($1{\rightarrow}6$)-${\beta}$-D-glucopyranosylester (HE) for the standardization of the shoot extract of AE as a health functional food ingredient. The quantitative analytical method of HE was optimized by HPLC analysis using reverse-phase C18 column at $40^{\circ}C$ with $H_2O$ and acetonitrile (70:30, v/v) as an isocratic mobile phase at a flow rate of 1.0 mL/min and detection wavelength of UV 205 nm. This HPLC/UV analytical method showed good specificity and high linearity in the tested range of 0.03125-2.0mg/ml with excellent coefficient of determination ($R^2$) of 0.9999. The limit of detection and limit of quantification were $12.0{\mu}g/mL$ and $36.5{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 0.2% and 0.1%, respectively. These results indicate that the established HPLC/UV analytical method is very simple, specific, precise, accurate, and reproducible and thus can be useful for the quantitative analysis of HE as a functional anti-hypertensive compound in AE extract.

• Korean Journal of Food Science and Technology
• /
• v.51 no.5
• /
• pp.420-424
• /
• 2019

An HPLC analysis method was developed and standardized for the detection of dieckol as a functional food ingredient in Ecklonia cava extracts. HPLC was performed using a Capcell Pak C18 column ($250{\times}4.6mm$, $5{\mu}m$) with a gradient elution of water and acetonitrile, both containing 0.1% (v/v) trifluoroacetic acid, at a flow rate of 1.0 mL/min at $25^{\circ}C$. The eluate was detected at 230 nm. For validation, the specificity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ) of dieckol were measured. The calibration curve for the detection of dieckol had high linearity ($R^2=0.9994$), with LOD and LOQ values of 0.38 and $1.16{\mu}g/mL$, respectively. Recovery of the quantified compound ranged from 99.61 to 100.71%. The relative standard deviation values of the intra-day and inter-day precisions were less than 1.7 and 1.25%, respectively. These results indicate that the reported HPLC method is simple, reliable, and reproducible for the detection of dieckol in Ecklonia cava extracts.

• Journal of Food Hygiene and Safety
• /
• v.34 no.1
• /
• pp.52-57
• /
• 2019

Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

• Journal of Korean Academy of Nursing
• /
• v.11 no.2
• /
• pp.83-104
• /
• 1981

Hemodialysis is essential treatment for the chronic renal failure patient's long-term cure and for the patient management before and after kidney transplantation. It sustains the endstage renal failure patient's life which didn't get well despite strict regimen and furthermore it becomes an essential treatment to maintain civil life. Bursing implementation in hemodialysis may affect the significant effect on patient's life. The purpose of this study was to obtain the basic data to solve the hypotension problem encountable to patient and the blood loss problem affecting hemodialysis patient'a anemic states by incomplete rinsing of blood in coil through all process of hemodialysis. The subjects for this study were 44 patients treated hemodialysis 691 times in the hemodialysis unit, The .data was collected at Gang Nam 51. Mary's Hospital from January 1, 1981 to April 30, 1981 by using the direct observation method and the clinical laboratory test for laboratory data and body weight and was analysed by the use of analysis of Chi-square, t-test and anlysis of varience. The results obtained an follows; A. On clinical laboratory data and other data by dialysis Procedure. The average initial body weight was 2.37 ± 0.97kg, and average body weight after every dialysis was 2.33 ± 0.9kg. The subject's average hemoglobin was 7.05±1.93gm/dl and average hematocrit was 20.84± 3.82%. Average initial blood pressure was 174.03±23,75mmHg and after dialysis was 158.45±25.08mmHg. The subject's average blood ion due to blood sample for laboratory data was 32.78±13.49cc/ month. The subject's average blood replacement for blood complementation was 1.31 ±0.88 pint/ month for every patient. B. On the hypotensive state and the coping approaches occurrence rate of hypotension was 28.08%. It was 194 cases among 691 times. 1. In degrees of initial blood pressure, the most 36.6% was in the group of 150-179mmHg, and in degrees of hypotension during dialysis, the most 28.9% in the group of 40-50mmHg, especially if the initial blood pressure was under 180mmHg, 59.8% clinical symptoms appeared in the group of“above 20mmHg of hypotension”. If initial blood pressure was above 180mmHg, 34.2% of clinical symptoms were appeared in the group of“above 40mmHg of hypotension”. These tendencies showed the higher initial blood pressure and the stronger degree of hypotension, these results showed statistically singificant differences. (P=0.0000) 2. Of the occuring times of hypotension,“after 3 hrs”were 29.4%, the longer the dialyzing procedure, the stronger degree of hypotension ann these showed statistically significant differences. (P=0.0142). 3. Of the dispersion of symptoms observed, sweat and flush were 43.3%, and Yawning, and dizziness 37.6%. These were the important symptoms implying hypotension during hemodialysis accordingly. Strages of procedures in coping with hypotension were as follows ; 45.9% were recovered by reducing the blood flow rate from 200cc/min to 1 00cc/min, and by reducing venous pressure to 0-30mmHg. 33.51% were recovered by controling (adjusting) blood flow rate and by infusion of 300cc of 0,9% Normal saline. 4.1% were recovered by infusion of over 300cc of 0.9% normal saline. 3.6% by substituting Nor-epinephiine, 5.7% by substituting blood transfusion, and 7,2% by substituting Albumin were recovered. And the stronger the degree of symptoms observed in hypotention, the more the treatments required for recovery and these showed statistically significant differences (P=0.0000). C. On the effects of the changes of blood pressure and osmolality by albumin and hemofiltration. 1. Changes of blood pressure in the group which didn't required treatment in hypotension and the group required treatment, were averaged 21.5mmHg and 44.82mmHg. So the difference in the latter was bigger than the former and these showed statistically significant difference (P=0.002). On the changes of osmolality, average mean were 12.65mOsm, and 17.57mOsm. So the difference was bigger in the latter than in the former but these not showed statistically significance (P=0.323). 2. Changes of blood pressure in the group infused albumin and in the group didn't required treatment in hypotension, were averaged 30mmHg and 21.5mmHg. So there was no significant differences and it showed no statistical significance (P=0.503). Changes of osmolality were averaged 5.63mOsm and 12.65mOsm. So the difference was smaller in the former but these was no stitistical significance (P=0.287). Changes of blood pressure in the group infused Albumin and in the group required treatment in hypotension were averaged 30mmHg and 44.82mmHg. So the difference was smaller in the former but there is no significant difference (P=0.061). Changes of osmolality were averaged 8.63mOsm, and 17.59mOsm. So the difference were smaller in the former but these not showed statistically significance (P=0.093). 3. Changes of blood pressure in the group iutplemented hemofiltration and in the Uoup didn't required treatment in hypotension were averaged 22mmHg and 21.5mmHg. So there was no significant differences and also these showed no statistical significance (P=0.320). Changes of osmolality were averaged 0.4mOsm and 12.65mOsm. So the difference was smaller in the former but these not showed statistical significance（P=0.199). Changes of blood pressure in the group implemented hemofiltration and in the group required treatment in hypotension were averaged 22mmHg and 44.82mmHg. So the difference was smatter in the former and these showed statistically significant differences (P=0.035). Changes of osmolality were averaged 0.4mOsm and 17.59mOsm. So the difference was smaller in the former but these not showed statistical significance (P=0.086). D. On the changes of body weight, and blood pressure, between the group of hemofiltration and hemodialysis. 1, Changes of body weight in the group implemented hemofiltration and hemodialysis were averaged 3.340 and 3.320. So there was no significant differences and these showed no statistically significant difference, (P=0.185) but standard deviation of body weight averaged in comparison with standard difference of body weight was statistically significant difference (P=0.0000). Change of blood Pressure in the group implemented hemofiltration and hemodialysis were averaged 17.81mmHg and 19.47mmHg. So there was no significant differences and these showed no statistically significant difference (P=0.119), But in comparison with standard deviation about difference of blood pressure was statistically significant difference. (P=0.0000). E. On the blood infusion method in coil after hemodialysis and residual blood losing method in coil. 1, On comparing and analysing Hct of residual blood in coil by factors influencing blood infusion method. Infusion method of saline 200cc reduced residual blood in coil after the quantitative comparison of Saline Occ, 50cc, 100cc, 200cc and the differences showed statistical significance (p < 0.001). Shaking Coil method reduced residual blood in Coil in comparison of Shaking Coil method and Non-Shaking Coil method this showed statistically significant difference (P < 0.05). Adjusting pressure in Coil at OmmHg method reduced residual blood in Coil in comparison of adjusting pressure in Coil at OmmHg and 200mmHg, and this showed statistically significant difference (P < 0.001). 2. Comparing blood infusion method divided into 10 methods in Coil with every factor respectively, there was seldom difference in group of choosing Saline 100cc infusion between Coil at OmmHg. The measured quantity of blood loss was averaged 13.49cc. Shaking Coil method in case of choosing saline 50cc infusion while adjusting pressure in coil at OmmHg was the most effective to reduce residual blood. The measured quantity of blood loss was averaged 15.18cc.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.44 no.1
• /
• pp.85-88
• /
• 2015

This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.

• Economic and Environmental Geology
• /
• v.49 no.6
• /
• pp.459-467
• /
• 2016

Due to the limited areal space for installation, borehole heat exchangers (BHEs) at depths deeper than 300 m are considered for geothermal heating and cooling in the urban area. The deep vertical closed-loop BHEs are unconventional due to the depth and the range of the typical installation depth is between 100 and 200 m in Korea. The BHE in the study consists of 50A (outer diameter 50 mm, SDR 11) PE U-tube pipe in a 150 mm diameter borehole with the depth of 300 m. In order to compensate the buoyancy caused by the low density of PE pipe ($0.94{\sim}0.96g/cm^3$) in the borehole filled with ground water, 10 weight band sets (4.6 kg/set) were attached to the bottom of U-tube. A thermal response test (TRT) and fundamental basic surveys on the thermophysical characteristics of the ground were conducted. Ground temperature measures around $15^{\circ}C$ from the surface to 100 m, and the geothermal gradient represents $1.9^{\circ}C/100m$ below 100 m. The TRT was conducted for 48 hours with 17.5 kW heat injection, 28.65 l/min at a circulation fluid flow rate indicates an average temperature difference $8.9^{\circ}C$ between inlet and outlet circulation fluid. The estimated thermophysical parameters are 3.0 W/mk of ground thermal conductivity and 0.104 mk/W of borehole thermal resistance. In the stepwise evaluation of TRT, the ground thermal conductivity was calculated at the standard deviation of 0.16 after the initial 13 hours. The sensitivity analysis on the borehole thermal resistance was also conducted with respect to the PE pipe diameter and the thermal conductivity of backfill material. The borehole thermal resistivity slightly decreased with the increase of the two parameters.