• Analytical Science and Technology
• /
• v.30 no.1
• /
• pp.20-25
• /
• 2017

An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

• Analytical Science and Technology
• /
• v.34 no.4
• /
• pp.180-190
• /
• 2021

This study compared the efficacy of chiral GC and chiral HPLC for the analysis of nicotine. To develop a suitable dispersive liquid-liquid microextraction (DLLME) method, the following parameters were optimized: pH, extraction solvent, dispersive solvent, type and quantity of salt, and laboratory temperature. The validation of the method was carried out by the established HPLC method. The LODs were 0.11 ㎍/mL and 0.17 ㎍/mL for the (S)- and (R)- enantiomers, respectively. The LOQs were 0.30 ㎍/mL and 0.44 ㎍/mL, respectively. The optimal calibration range was between 0.30-18 ㎍/mL and 0.44-4.40 ㎍/mL, respectively, and the correlation coefficient (r²) was 0.9978-0.9996. The intra-day accuracy was 79.9-110.6 %, and the intra-day precision was 1.3-12.0 %. The inter-day accuracy was 87.8-108.0 %, and the inter-day precision was 4.0-12.8 %. E-liquid and biological fluids (urine and saliva) were analyzed using the established method.

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.370-376
• /
• 2015

An analytical method for determining phenol considered priority pollutants of the US EPA and precursor of toxic phenolic compounds by solid-phase extraction (SPE) and high performance liquid chromatographic systems (HPLC) equipped with fluorescence and mass selective detectors have been developed. The SPE process for sample preconcentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of pH, elution solvent, and elution volume on the recoveries of the analytes were investigated with HPLC/FLD. Average recovery of >87.0% was achieved with 60 mg sorbents using 5 mL of methanol as an elution solvent at pH=3.

• Natural Product Sciences
• /
• v.17 no.4
• /
• pp.321-327
• /
• 2011

In this study, quantitative analysis was developed using HPLC/UVD for the quality evaluation of Scutellariae Radix. For quantitative analysis, six major bioactive compounds were assessed. The separation conditions employed for HPLC/UVD were optimized using Phenomenex $C_{18}$ column ($250{\times}4.6$ mm, 5 ${\mu}m$) with a gradient of solvent A (1% acetic acid of $H_2O$) and solvent B (acetonitrile : methanol : acetic acid = 70 : 30 : 1) as the mobile phase at a flow rate of 1.0 mL/min and a detection wavelength of 275 nm. These methods were fully validated with respect to linearity, accuracy, precision and recovery. The HPLC/UVD method was applied successfully to the quantification of six major compounds in the extract of Scutellariae Radix. The results indicate that the established HPLC/UVD method is suitable for the quantitative analysis and quality control of multicomponents in Scutellariae Radix.

• Korean Chemical Engineering Research
• /
• v.53 no.6
• /
• pp.717-722
• /
• 2015

D-limonene included in citrus fruits is obtainable to extract essential oil as well as separate the oil ingredient. Soxhlet extraction, a type of SDE (Simultaneous steam Distillation and solvent Extraction), was used to extract limonene from tangerine peel. HPLC analysis was performed to quantify extracted d-limonene by using reversed-phase HPLC column. Results of HPLC analysis showed that the optimal extraction time was 2 hours in any solvent, and the extracted amounts of d-limonene in tangerine peel (per g tangerine peel) were 7.77 mg, 0.49 mg, and 0.28 mg in ethyl alcohol, n-hexane, and ether. Because yield was the highest in using ethyl alcohol as a solvent, polarity is stronger factor to effect on yield of extraction than boiling point.

• Food Science and Preservation
• /
• v.22 no.4
• /
• pp.553-558
• /
• 2015

The aims of this study was to optimize the extraction conditions of sinigrin from Dolsan leaf mustard. Dolsan leaf mustard (Dolsan-eup, Yeosu-si) harvested during at May 2014 was used for sinigrin extraction. After the extraction of sinigrin using 50% $CH_3CN$, 10% $NH_4Cl$, 60% $CH_2OH$, and 70% $CH_3OH$, the sinigrin content was measured by HPLC analysis. The results showed that sinigrin content was highest with 50% $CH_3CN$ solvent extraction and UV detector sensitivity was greater at 228 nm rather than at 242 nm. The sinigrin concentrations of leaf, stem and root with 50% $CH_3CN$ extraction were 345 ppm, 728 ppm, and 539 ppm, respectively. After extraction of the different parts of Dolsan leaf mustard, The standard retention time by HPLC analysis of sinigrin content was 2.054, 2.032, 2.059, and 2.035 min from the root, stalk, and leaf, respectively. On the other hand, HPLC analysis showed that the leaf extracts contained glucoraphanin, one of glucosinolates. The optimum time and extraction solvent for the sinigrin extraction from Dolsan leaf mustard was found to be 24 hr with 50% $CH_3CN$ solvent. In addition, opotimum UV detector k at 228 nm. These results showed that the optimum extraction conditions for Dolsan leaf mustard were 24 hr extraction with 50% $CH_3CN$ solvent. In addition, the optimum wavelength of UV detector was determined to be 228 nm for sinigrin analysis. Therefore, this study could provide a useful information for sinigrin extraction and its systematic analysis during the storage.

• Journal of Food Hygiene and Safety
• /
• v.13 no.4
• /
• pp.344-354
• /
• 1998

This study was conducted to evaluate the MSPD and HPLC method about simultaneous determination for residual synthetic antimicrobials of sixteen species such as sulfonamide etc. in livestock products. Elution solvent used in HPLC was ethylacetate:acetonitrile (4:1), and mobile phases for solvent A and B were water:methanol:acetonit rile:phosphric acid (700:250:50:0.2) and 100% acetonitrile respectively. The detector and absorbency used in HPLC was UV 266 nm. This study showed the reduction effect of 99.1% for organic solvents, 94% for experimental steps, 95% for analytical time and manpower and 98.9% for costs compared with korea food standard method. The average recovery rates for chicken, bovine, pork and milk were 67.7% 96.2%, 67.7%~96.6%, 70.0%~96.2%, and 13.8%~97.8%.

• The Journal of Korean Medicine
• /
• v.31 no.6
• /
• pp.8-15
• /
• 2010

Objectives: We investigated to develop and validate HPLC-PDA methods for simultaneous determination of eight constituents in Galgeun-tang (GGT). Methods: Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 230 nm, 254 nm, and 280 nm, were used for quantification of the eight marker components of GGT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Results: Calibration curves were acquired with $r^2$ > 0.9999, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each component was in the range of 87.33-101.38%, with an RSD less than 7.0%. The contents of the eight components in GGT were 1.98-12.17 mg/g. Conclusions: The established method will be applied for the quantification of marker components in GGT.

• Herbal Formula Science
• /
• v.18 no.1
• /
• pp.95-103
• /
• 2010

Objectives : To develop and validate HPLC-PDA methods for simultaneous determination of seven constituents in Samsoeum(SSE). Methods : Reverse-phase chromatography using a Gemini C18 column operating at $40^{\circ}C$, and photodiode array(PDA) detection at 254 and 280 nm, were used for quantification of the seven marker components of SSE. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Results : Calibration curves were acquired with $r^2$>0.9997, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 3.0%. The recovery rate of each compound was in the range of 100.07-112.65%, with an RSD less than 4.0%. The contents of seven compounds in SSE were 1.24-10.53 mg/g. Conclusions : The established method will be helpful to improve quality control of SSE.

• 한국생물공학회:학술대회논문집
• /
• 2005.10a
• /
• pp.566-569
• /
• 2005

A novel purification method was developed for producing homoharringtonine from Cephalotaxus koreana, to guarantee high purity and yield. Our simple, efficient procedure for isolating and purifying homoharringtonine from C. koreanabiomass consisted of solvent extraction, synthetic adsorbent treatment, low-pressure chromatography, followed by high performance liquid chromatography (HPLC). The use of active clay treatment and silica gel low-pressure chromatography in the pre-purification process allowed for the rapid, efficient separation of homoharringtonine from interfering compounds and dramatically increased the yield and purity of crude homoharringtonine for high-performance liquid chromatography (HPLC) purification steps compared with alternative processes. Homoharringtonine could be obtained simply with high yield and purity from biomass using this purification method, while minimizing solvent use and the scale and complexity of HPLC operations for homoharringtonine purification. Purified homoharringtonine was identified and characterized.