• Journal of the Korean Society of Tobacco Science
• /
• v.31 no.1
• /
• pp.45-50
• /
• 2009

In this study, a simple gradient RRLC method for rapid determination of carbonyl compounds of cigarette smoke was developed. Within 10 min, 8 carbonyl compounds have been separated and identified on ZORBAX Eclipse XDB-C18 column ($4.6{\times}50\;mm$, $1.8\;{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. RRLC was used for the quantification of carbonyl compounds in mainstream smoke of 3R4F reference cigarette, and evaluated those efficiencies in the recovery, repeatability and reproducibility. The correlation coefficients ($r^2$) for calibration curves of carbonyl compounds were over 0.9998. The developed RRLC method was successfully applied to the analysis of smoke samples and the recoveries of carbonyl compounds were in the range of 97.5~102.1% with RSD<3.1%.

• Natural Product Sciences
• /
• v.18 no.2
• /
• pp.83-88
• /
• 2012

In order to facilitate the quality control of the fruits of Crataegus pinnatifida, a simple, accurate and reliable HPLC method was developed for the simultaneous determination of the three bioactive compounds: chlorogenic acid (1), rutin (2), and hyperin (3), which were selected as the chemical markers of C. pinnatifida. Separation was achieved on an Agilent Eclipse XDB-C18 column with a gradient solvent system of 0.1% trifluoroacetic acid aqueous-acetonitrile at a flow-rate of 1.0 mL/min and detected at 254nm. All three calibration curves showed good linearity ($R^2$ > 0.998). The recoveries of three marker compounds were in the range of 94.87~111.52 %. The contents of chlorogenic acid (1), rutin (2), and hyperin (3) of the fruits of C. pinnatifida collected from 23 district markets in Korea, Japan, and China were 0.16~0.65 mg/g, 0.07~1.24 mg/g, and 0.03~0.62 mg/g, respectively. The results demonstrated that this method is simple and reliable for the quality control of the fruits of C. pinnatifida.

• Natural Product Sciences
• /
• v.20 no.3
• /
• pp.182-190
• /
• 2014

An ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was established for quantitative analysis of twelve components, allantoin (1), morroniside (2), 5-hydroxymethyl-2-furfural (5-HMF) (3), loganin (4), coumarin (5), cinnamic acid (6), mesaconitine (7), cinnamaldehyde (8), hypaconitine (9), aconitine (10), alisol B (11), and alisol B acetate (12) in a Palmijihwang-hwan decoction. The twelve constituents were separated on a UPLC BEH C18 column ($2.1{\times}100mm$, $1.7{\mu}m$) at a column temperature of $40^{\circ}C$ by gradient elution with 0.1% (v/v) formic acid in water and acetonitrile as the mobile phase. The flow rate was 0.3 mL/min and the injection volume was $2.0{\mu}L$. Calibration curves of all compounds were acquired with values of the correlation coefficient ${\geq}0.99$ within the test ranges. The limits of detection and quantification for all analytes were 0.01 - 4.53 ng/mL and 0.03 - 13.60 ng/mL, respectively. The concentrations of the compounds 1 - 9 and 12 were 72.83, 4389.00, 4859.00, 3155.17, 223.67, 33.50, 1.97, 518.00, 2.25, and $25.00{\mu}g/g$, respectively. However, compounds 10 and 11 were not detected.

• Korean Journal of Pharmacognosy
• /
• v.51 no.2
• /
• pp.139-145
• /
• 2020

The leaves of Diospyros kaki Thunb. were used to treat heart disease and hypotension in traditionally East Asia. The purpose of this study is to simultaneously quantitiative analyze the content of flavonoids in leaves of D. kaki. The isolated flavonoids from the leaves of D. kaki, and the structure of the isolated flavonoids were analyzed based on ¹H and ¹³C NMR spectrum compared to literature data. Simultaneous quantitative analysis of the isolated flavonoids was validated using high performance liquid chromatography (HPLC). Results showed that the calibration curves of the flavonoid compounds were confirmed that they have a large linearity with a correlation coefficient (R²) of 0.99. In the intra-day and inter-day analysis, accuracy and precision of five compounds were measured that accuracy was 94.39 to 114.47% and precision was less than 3.00%. Content analysis showed hyperoside (1.30 ± 0.09%), astragalin (0.81 ± 0.06%), trifoline (1.58 ± 0.07%), quercetin (0.13 ± 0.02%) and kaempferol (1.33 ± 0.25%).

• Natural Product Sciences
• /
• v.12 no.4
• /
• pp.237-240
• /
• 2006

Paeoniflorin, the major component of the root of Paeonia lactiflora, was quantitatively analyzed using $^1H-NMR$ spectrometry. The quantity of paeoniflorin was calculated by the ratio of the intensity of the signals (H-9, H-10, H-2', 6') to the aldehyde peak of the known amount of internal standard, 2,4,6-trihydroxybenzaldehyde. These results were compared with the conventional HPLC method. The contents of paeoniflorin in P. lactiflora, which were respectively calculated by H-9, H-10, H-2', 6' in the $^1H-NMR$ spectra and HPLC, were determined $2.60{\pm}0.07,\;2.44{\pm}0.09,\;2.77{\pm}0.12\;and\;2.46{\pm}0.16%$. The advantages of quantitative $^1H-NMR$ analysis are that can be analyzed to identify and quantify, and no reference compounds required for calibration curves. Besides, it allows rapid and simple quantification for paeoniflorin with an analysis time for only 20 min without any preprocessing.

• Korean Journal of Veterinary Service
• /
• v.26 no.2
• /
• pp.157-162
• /
• 2003

This stud was attempted to detect six benzimidazoles[thiabendazole(TBZ), oxfendazole(OFZ), mebendazole(MBZ), flubendazole(FLBZ), albendazole(ABZ), and febendazole(FBZ)] in eggs using high performance liquid chromatography(HPLC) with photodiode array detector(DAD) simultaneously. The eluates were determined by HPLC on a waters X-Terra$^{TM}\;C_{18}$ reverse-phase column($4.6{\times}250nm,\;5{\mu}m$) with DAD at 295nm. The mobile phase was 0.04M ammonium phosphate(pH 7.5)/ACN(62.28 v/v) run isocratically. The calibration curves were linear(r>0.999) for six benzimidazoles. Average recovery rate from eggs were 94.54% for TBZ, 97.71% for OFZ, 88.82% for MBZ, 93.71% for FLBZ, 78.61% for ABZ, and 75.09% for FBZ, respectively. The limits of detection and quantification were 2.27ppb, 3.88 for TBZ, 9.34ppb, 15.61ppb for OFZ, 28.53ppb, 45.15ppb for MBZ, 27.39ppb, 40.95ppb for FBZ, 8.61ppb, 13.95ppb for ABZ and 12.79ppb, 22.34ppb for FBZ, respectively.

• Korean Journal of Food Science and Technology
• /
• v.4 no.1
• /
• pp.24-28
• /
• 1972

Synthetic food preservatives were analysed in foods collected in Seoul area on Aug. 10, 1971. Sorbic acid, benzoic acid, dehydroacetic acid and butyl p-hydroxybenzoate were determined by the simultaneous gas chromatography using FID at $200{\circ}C$ and a column of Chromosorb W coated with 5% $DGS{\sim}1%\;H_3PO_4$. The recovery rates of each preservative were from 76.7% to 96.3%. The calibration curves show linearity within a range from 0.3 to $2.5{\mu}g$ of standard preservatives. The results obtained were as follows: 1) Benzoic acid was used as well as butyl p-hydroxybenzoate in soy. 2) Sorbic acid was not found in soy. 3) From all breads and biscuits benzoic acid was found as trace. 4) Detected preservatives were below the range of permitted limit. 5) From 2 soy among 15 samples dehydroacetic acid was found.

• Analytical Science and Technology
• /
• v.8 no.3
• /
• pp.365-370
• /
• 1995

A tissue biosensor for the measurement of dopamine has been constructed by immobilizing the slice of Sprague-Dawley rat liver on $NH_3$-sensing electrode. To overcome the defect of tissue sensors, the maximal velocity of response curve was measured and applied to the Lineweaver-Burk equation instead of the Nernst equation. And then compared the results with those obtained from Nernst equation. When we obtained calibration curves from Nernst equation, there were variances on the slope and the linear range. But from Lineweaver-Burk equation, the scale of variance was small. Response time was reduced from 7~12 minutes to 2~3 minutes.

• Analytical Science and Technology
• /
• v.30 no.5
• /
• pp.221-225
• /
• 2017

Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

• Bulletin of the Korean Chemical Society
• /
• v.35 no.1
• /
• pp.211-217
• /
• 2014

A new needle-based device for headspace wire coated in-needle microextraction (HS-WC-INME) was fabricated using a nichrome wire coated with poly(ethylene glycol) (PEG) and poly(dimethylsiloxane) (PDMS) mixture. The proposed needle device was applied for the determination of volatile compounds in lavender and lavandin essential oils by gas chromatography. Fundamental parameters such as needle design, conditions of extraction and desorption were optimized along with the validation of the extraction and desorption efficiency. The optimal conditions were 30 min extraction at $50^{\circ}C$ and 2 min desorption at $240^{\circ}C$. The calibration curves showed good linearity with the suitable values of the coefficients of determination ($r^2$) greater than 0.99. The limits of detection for linalyl acetate, ${\beta}$-caryophyllene, linalool and (+)-limonene were 7.15, 9.04, 10.79 and 22.26 ng, respectively. Analytical recoveries were acceptable in the test samples, varying from 86.7% to 108.0%. The values of relative standard deviations for run to run showed range less than 0.9% while 3.9% through 7.2% for needle to needle. The proposed PEG-PDMS coating could be more suitable than PDMS coating to extract particular polar groups such as alcohols.