• Korean Journal of Fisheries and Aquatic Sciences
• /
• v.43 no.4
• /
• pp.293-297
• /
• 2010

To prevent amnesic shellfish poisoning (ASP) resulting from the consumption of shellfish contaminated with domoic acid, the quantitative analysis of domoic acid is very important. We validated a high performance liquid chromatography (HPLC) method for accurate and precise quantification of domoic acid. A clear peak and the isolation of domoic acid resulted on injecting a 50% methanol extract of CRM-ASP-Mus-c mussel reference material using HPLC. The limit of detection of domoic acid under the established HPLC conditions was $0.10\;{\mu}g/g$, and the limit of quantification of the toxin under the same conditions was $0.25\;{\mu}g/g$. The intra-accuracy and precision for domoic acid in CRM-ASP-Mus-c were 90.7-95.7% and 0.28-22.25%, respectively. The inter-accuracy and precision for domoic acid were 89.1-97.1% and 1.7-4.1%, respectively. The mean recovery of domoic acid in methanol extracts from ten species of marine invertebrates was 88.6-1105.1%.

• Korean Journal of Pharmacognosy
• /
• v.43 no.4
• /
• pp.286-290
• /
• 2012

Many diterpenoids from Siegesbeckia species (Compositae) and their anti-inflammatory actions have been examined. In this research, high-performance liquid chromatography-ultraviolet spectrophotometer (HPLC-UV) method was used to compare the quantitative level of kirenol (ent-pimarane-type diterpenoid) in the aerial parts of Korean S. glabrescens and S. pubescens and the Chinese Siegesbeckiae Herba. Fingerprints of the two HPLC chromatograms of Korean S. glabrescens and S. pubescens were similar, but considerably different from Chinese Siegesbeckiae Herba. The content of kirenol in S. pubescens ($16.51{\pm}0.10$ mg/ml dry weight as mean${\pm}$RSD) was higher than S. glabrescens ($13.48{\pm}0.12$ mg/g dry weight). These values were considerably higher than the Chinese Siegesbeckiae Herba ($1.55{\pm}0.74$ mg/g dry weight). Thin layer chromatography (TLC) analysis demonstrated the containing of kirenol in the three plant materials, but the presence of siegeskaurolic acid (entkaurane-type diterpenoid) only in the Chinese Siegesbeckiae Herba.

• Korean Journal of Environmental Agriculture
• /
• v.23 no.4
• /
• pp.251-257
• /
• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• Journal of Microbiology and Biotechnology
• /
• v.16 no.4
• /
• pp.643-646
• /
• 2006

Because of potential health hazards of aflatoxins for humans, the present study was conducted to monitor aflatoxin $B_1\;(AFB_1)$ in livestock feeds. A total of 249 samples of feeds collected in Korea were analyzed by DC-ELISA for qualitative analysis of $AFB_1$. Then, 27 samples that were verified to contain $AFB_1$ by DC-ELISA were quantitated by HPLC/FLD. HPLC/FLD analysis revealed that only one sample collected from a farm contained 11 ppb of $AFB_1$, whereas the other samples collected from feed companies did not contain $AFB_1$. The presence of $AFB_1$ was further confirmed by LC/MS analysis. TLC analysis indicated that the result of the DC-ELISA was most likely due to possible contamination of other mycotoxins rather than $AFB_1$. In conclusion, HPLC/FLD analysis following DC-ELISA is necessary for rapid and accurate detection of $AFB_1$.

• Journal of the Korea Academia-Industrial cooperation Society
• /
• v.15 no.1
• /
• pp.396-401
• /
• 2014

In this study, we used NIR spectrum method instead of conventional HPLC method to shorten the analysis and manufacturing time of the loxoprofen products. Loxoprofen mixtures with other pharmaceutical additives were prepared and evaluated by the NIR spectrometer and the HPLC system. Validation of both methods was performed for specificity, accuracy and precision. NIR spectrometer method was validated and revealed proper results for the in-process quality control in the pharmaceutical field. In conclusion, NIR spectrometry can be replaced by HPLC method.

• Analytical Science and Technology
• /
• v.23 no.1
• /
• pp.97-101
• /
• 2010

(R)-N-3,5-dinitrobenzoyl (DNB) phenylglycinol derived chiral selector was used as a HPLC chiral stationary phase (CSP) for the resolution of racemic N-acylnaphthylalkylamines. In this study, determination of optical purity was performed by both chiral chromatography and NMR spectroscopy by using the (R)-phenylglycinol derived chiral selector. The data of accuracy and precision of each optical purity value are calculated from the results of NMR and HPLC experiments by comparing with true value. Average error of the NMR method was +2.2% with average RSD of 4.54%, while that of HPLC method was -3.5% with average RSD of 3.23%.

• Journal of the Korean Chemical Society
• /
• v.45 no.6
• /
• pp.524-531
• /
• 2001

Micro-HPLC/IS/MS after solid phase extraction has been employed to enhance the accu-racy in the determination of toxic microcystins, such as microcystin-LR, -YR and -RR. The absorbance at 238 nm in HPLC/UV and characteristic spectra of 135 m/z and $[M+H]^+$ m/z in MS have been widely monitored to identify those microcystin-LR, -YR and -RR. In this study, new lines at 507 m/z for LR, 520 m/z for RR and 532 m/z for YR have been additionally detected in the micro-HPLC/IS/MS spectrum, corresponding to double charge. The micro-HPLC/IS/MS methodology has been applied to investigate the presence of the toxic microcystins in Taecheong lake.

• Journal of Life Science
• /
• v.34 no.1
• /
• pp.59-67
• /
• 2024

LS-RUG-com preparation in a complex extract from mixture of three natural plants. Rubus crataegifolius/unriped, Gardenia jasminoides and Ulmus marcrocarpa that have been widely used in traditional functional health food. This study was conducted to establish the HPLC analysis methods that can be used to establish quantitative analysis of R. crataegifolius, G. jasminoides and U. macrocarpa for standardization of LS-RUG-com preparations. HPLC analysis methods for simultaneous determination of ellagic acid and geniposide and single determination of catechin-7-O-β-D-apiofuranoside were established for the quality control of natural plants complex (LS-RUG-com). Validation of HPLC analysis were performed by checking specificity, accuracy, precision, limit of detection and quantitation, and linearity following ICH (International Council for Harmonisation) guideline. As the result of quantitative analysis, the contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in each plant extracts were 11.2 mg/g (ellagic acid) and 72 mg/g (geniposide) and 10.2 mg/g (catechin-7-O-β-D-apiofuranoside). The contents of ellagic acid, geniposide and catechin-7-O-β-D-apiofuranoside in LS-RUG-com were 4.62~6.82 mg/g (ellagic acid), 19.2~28.8 mg/g (geniposide) and 1.36~2.04 mg/g (catechin-7-O-β-D-apiofuranoside) respectively.

• Applied Chemistry for Engineering
• /
• v.9 no.3
• /
• pp.404-406
• /
• 1998

Analysis for the imidazoline type cationic surfactants was performed by the gas chromatography(GC) and high performance liquid chromatography(HPLC). The composition of the alkyl chain distribution was investigated by GC after base/Acid hydrolysis of the imidazoline ring. The distribution of total alkyl chain was separated clearly by a Bondclone C18/NOVA-Pak C18 HPLC column using 50% acetonitrile in methanol containing 0.1M sodium perchlorate as a mobile phase. Alkyl chain distribution and average molecular weight of imidazoline type cationic surfactants were obtained based on these analytical methods. The agreement of results from GC and HPLC was good. The detection limit of imidazoline by HPLC method was 10ng without pretreatment.

• The Korea Journal of Herbology
• /
• v.22 no.2
• /
• pp.97-102
• /
• 2007

Objectives : This study presents a high performance liquid chromatography - electrospray ionization-mass spectrometer (HPLC-MS/MS) methods for the quantitative and qualitative analysis of various active components in Samul-tang, which is composed of four crude herbs. Methods : HPLC-ESI-MS/MS for the determinations of paeoniflorin and 5-HMF (5-hydroxymethyl 2-furaldehyde) in the Samul-tang, the separation method was performed on an COSMOS1L 5C18-AR-Il (2.0 X 150 mm I.D.) column by gradient elution with 0.1% acetic acid and 5% CH3CN in water (A)-0.1% acetic acid and 5% H20 in CH3CN (B) as the mobile phase at a flow-rate of 300 ${\mu}L/min$ with detection at quadrupole mass spectrometer. The all marker substances were always detected as the base peaks in the positive ion mode. Results : The paeoniflorin of Paeoniae Radix in Samul-tang showed a strong base peak [M+H2O]+ in the positive detection mode to give the following as; paeoniflorin (498.109 [M+H2O]+, 479.8 [M]+, 301 [M-glucose]+, 179.3 [glucose]+). Based on the HPLC retnetion time and MS of standard compounds confirmed the identity of active compounds in Rehmanniae Radix Preparata as follows; 5-HMF (127.0[M+H]+, 109.3 [M-OH]+) in the positive ion mode. Conclusion : According to the above results, HPLC-ESI-MS method permits assignment of tentative structures such as paeoniflorin and 5-HMF in the Samul-tang.