• Archives of Pharmacal Research
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• v.27 no.12
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• pp.1202-1206
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• 2004

A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/ MS) method for the determination of lithospermic acid B (LSB) in rat serum was developed. LSB and internal standard, 7-hydroxy-3-phenyl-chromen-4-one (HPC) were extracted from rat serum with methyl-tert-butyl ether at acidic pH and analyzed on a Luna $C_8$ column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 6.5) (50:50, v/v). The analytes were detected using a negative electrospray ionization tandem mass spectrometry in the multiple- reaction-monitoring mode. The standard curve was linear $(r^2 = 0.997)$ over the concentration range of 10.0-500 ng/mL. The coefficient of variation and relative error for intra- and interassay at three QC levels were 1.1~6.2% and -10.3~-2.7%, respectively. The recovery of LSB from serum sample ranged from 73.2 to 79.5%, with that of HPC (internal standard) being 75.1 %. The lower limit of quantification for LSB was 10 ng/mL using 50 ${\mu}L$ of serum sample.

• Archives of Pharmacal Research
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• v.25 no.5
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• pp.613-616
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• 2002

A high-performance liquid chromatographic method has been developed for the separation and quantification of chrysin and synthetic chrysin derivatives (12 chrysin alkyl and 7 chrysin acyl derivatives). The chromatography was performed using a $Nova-Pak^{\circledR}C_{18}$ column. A RP-HPLC was performed by using a binary mixture (MeOH-10 mM H$_3$PO$_4$) as a mobile phase, and the column temperature was maintained at room temperature. A flow rate was 1.0 ml/min, and the effluent was monitored at a wavelenth of 280 nm. The retention times for chrysin acyl and alkyl derivatives were within 10 minutes and 20 minutes, respectively. The absolute recovery of samples were all over 96%. The detection limits were 0.1~18 ng at S/N = 3 ratio.

• Korean Journal of Veterinary Service
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• v.30 no.3
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• pp.421-428
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• 2007

This study was conducted two kinds of aims: 1) to modify the analytical methods (conditions) by high performance liquid chromatography - fluorescence detector for the detection of residual ivermectin in raw milk, 2) to provide basic information for the evaluation of standard of the residual ivermectin in raw milk. It could be considerable that negative ion spectra can be better method in the LC/MS analysis for the detection of residues, Characteristic daughter ions were observed in negative ion spectra, however, linear line was not formed in positive ion one. Three Holstein cows ($500{\pm}10kg$) were applied to commercial ointment of ivermectin just one time at the first day of test, and residues in raw milk were examined for 20day after administration. The limit of detection (LOD) was 0.65ng (n=5) by HPLC/FLD, and recovery rates were $87.85%{\sim}99.47%$. The peak was observed at the 4th day, and residues lasted to the end. Thus ivermectin was prohibited when lactating.

• Food Science of Animal Resources
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• v.34 no.6
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• pp.749-756
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• 2014

A rapid and simple analytical method for L-carnitine was developed for infant and toddler formulas by liquid chromatography tandem mass spectrometry (LC-MS/MS). A 0.3 g of infant formula and toddler formula sample was mixed in a 50 mL conical tube with 9 mL water and 1 mL 0.1 M hydrochloric acid (HCl) to chemical extraction. Then, chloroform was used for removing a lipid fraction. After centrifuged, L-carnitine was separated and quantified using LC-MS/MS with electrospray ionization (ESI) mode. The precursor ion for L-carnitine was m/z 162, and product ions were m/z 103 (quantitative) and m/z 85 (qualitative), respectively. The results for spiked recovery test were in the range of 93.18-95.64% and the result for certified reference material (SRM 1849a) was within the range of the certificated values. This method could be implemented in many laboratories that require time and labor saving.

• YAKHAK HOEJI
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• v.36 no.5
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• pp.506-511
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• 1992

The Prostaglandins were derivatized rapidly with monodansyl cadaverine as a fluorophore in mild conditions. The carboxylic moiety of prostaglandins was activated with diethyl phosphorocyanidate and successively coupled with fluorophore in dimethylformamide at room temperature. The labeling yield was reached about 95% at 15 min using arachidic acid $(C_{20:0})$ as a test sample. This derivative showed constant fluorescent intensity at $4^{\circ}C$ for 180 days. The derivatives of prostaglandins were shown high solvent selectivity with tetrahydrofuran in reversed-phase column. therefore, these derivatives could be successfully separated on YMC pack A-212(S-5 120A C8) column in tetrahydrofuran-based eluents. The detection limits of these derivatives was ca. 500 fmol and determination limits was ca. 5 pmol as injected amount in fluorescent detection $({\lambda}ex.\;340\;nm,\;{\lambda}em.\;520\;nm)$. In this method, the ranges of recovery and coefficient of variation were $93.6{\sim}102.7%$ and $4.3{\sim}5.8%$, respectively.

• Journal of the East Asian Society of Dietary Life
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• v.16 no.5
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• pp.585-591
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• 2006

We report a novel HPLC method for analyzing the capsaicinoids and nonivamide. The following conditions were used: a total column and column temperature of $3^{\circ}C$, a detection wavelength of 280 nm, an eluent containing acetonitrile : 0.5% formic acid(31:69, v/v). The experimental data was compared with standard nonivamide and capsaicin. The results showed that nonivamide was eluted in 96.7 minutes with a recovery ratio of 96.5% after adding known nonivamide. In addition, the detection limit for nonivamide was 18.6 ng. The capsaicinoids from Korean pepper were extracted (after blooming 60th) from 3 breeds cultivated in Korea, Buchon, Chungyang and Hanbando. and crisis it analyzed sympathizes the nonivamide in the result nonivamide from the Buchon and the Chungyang which are not detected from the Hanbando $0.16{\sim}0.24{\mu}g/g$ it detects with very small amount it contains it confirmed the each capsaicinoid with the HPLC and the LC-MS. These results are expected contribute to the quality control of various product processes, which includes product delivery inspection as well as examining the capsaicinoids present in the product for possible medicine manufacture and various foodstuff, and the nonivamide content, which may be a feed for various manufacturing processes involving chemical synthesis.

• Journal of agriculture & life science
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• v.46 no.6
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• pp.165-171
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• 2012

As a preceding study for investigating the influence of sound wave stimulus on Arabidopsis thaliana metabolomics, the polar secondary metabolomes of the plant were determined using high performance liquid chromatography coupled with tandem mass spectrometry. A total of 10 polar secondary metabolomes were characterized and quantified. Among them, 4 metabolomes, p-coumaroylagmatine isomer (7 and 8), p-coumaroylagmatine isomer (9 and 10) were identified in the plant for the first time. The validation was conducted in terms of linearity, recovery, precision, limit of detection (LOD) and limit of quantification (LOQ). The validated method was applied to the simultaneous quantification of the 10 polar secondary metabolomes.

• Nuclear Engineering and Technology
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• v.49 no.5
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• pp.928-940
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• 2017

An experiment using the $Prim{\ddot{a}}rkreisl{\ddot{a}}ufe$ Versuchsanlage (PKL) was performed for the OECD/NEA PKL-3 Project as a counterpart to a previous test with the large-scale test facility (LSTF) on a cold leg smallbreak loss-of-coolant accident with an accident management (AM) measure in a pressurized water reactor. Concerning the AM measure, the rate of steam generator (SG) secondary-side depressurization was controlled to achieve a primary depressurization rate of 200 K/h as a common test condition; however, the onset timings of the SG depressurization were different from each other. In both tests, rapid recovery started in the core collapsed liquid level after loop seal clearing, which caused whole core quench. Some discrepancies appeared between the LSTF and PKL test results for the core collapsed liquid level, the cladding surface temperature, and the primary pressure. The RELAP5/MOD3.3 code predicted the overall trends of the major thermal-hydraulic responses observed in the LSTF test well, and indicated a remaining problem in the prediction of primary coolant distribution. Results of uncertainty analysis for the LSTF test clarified the influences of the combination of multiple uncertain parameters on peak cladding temperature within the defined uncertain ranges.

• Mass Spectrometry Letters
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• v.9 no.4
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• pp.95-99
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• 2018

An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

• Journal of Preventive Veterinary Medicine
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• v.42 no.4
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• pp.171-176
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• 2018

A study of the tissue depletion of florfenicol (FFC) administered orally to pigs at a dose of 0.05 kg/ton feed for 7 days was performed. Sixteen healthy cross swine were administered with FFC. Four treated animals were arbitrarily selected to be sacrificed 1, 3 and 5 days after the end of treatment. FFC residue concentrations in muscle, liver, kidney, and fat were determined using high-performance liquid chromatography (HPLC) with ultraviolet photometric detector at 230 nm. The correlation coefficient ($R^2$) of the calibration curve for florfenicol amine (FFCa) was > 0.997 and the limits of detection and quantification were 0.012 and $0.040{\mu}g/mL$, respectively. Recovery rates in swine edible tissues ranged from 79.1 to 93.5%. In the FFC-treated group, FFC residues at 3 days post-treatment were below the maximum residue limits (MRLs) in muscle, kidney and fat, and those at 5 days post-administration were below the MRLs in all edible tissues. These results suggest that the withdrawal period of FFC after the drug treatment might be 5 days, which is a sufficient amount of time for reduction of the FFC residues below the MRLs in all edible tissues.