• Natural Product Sciences
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• 제16권2호
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• pp.116-122
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• 2010

A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of five representative metabolites of the iridoid and phenolic classes from Rehmannia glutinosa. The optimal chromatographic conditions were obtained on an ODS column (5 mm, $4.6{\times}250\;mm$) with the column temperature at $25^{\circ}C$. The mobile phase was composed of water and acetonitrile using a gradient elution with the flow rate 0.3 mL/min. Detection wavelength was set at 205 nm. All calibration curves showed good linear regression ($r^2$ > 0.997) within test ranges. Limits of detection (LOD) and quantitation (LOQ) values were lower than 0.123 and $0.373\;{\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.09 - 0.76% and 0.16 - 1.41%, respectively, and the overall recoveries of 99.03 - 102.67% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytic method. The verified method was successfully applied to the quantitative determination of five representative metabolites in twenty-one commercial Rehmannia glutinosa samples from different markets in Korea and China. The analytical results showed that the contents of the five analytes vary significantly with sources.

• Natural Product Sciences
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• 제18권3호
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• pp.158-165
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• 2012

A UPLC method for the simultaneous determination of seven compounds was established for the quality control in H. cordata. The UPLC was performed on a $C_{18}$ HSS T3 $2.1{\times}100$ mm, 1.8 ${\mu}m$ column during a 13 minute gradient elution of 0.2% aqueous acetic acid and acetonitrile with the flow rate of 0.2 mL/min at $30^{\circ}C$. The UPLC method was validated according to the ICH guideline of analytical procedures with respect to precision, accuracy, and linearity. The limit of determination and quantitation for the seven compounds were 0.01-0.09 and 0.03-0.28 ${\mu}g/mL$, respectively. The calibration curves of all seven compounds showed good linearity ($r^2$ > 0.999). The intra-day and inter-day the RSD values used to evaluate the precision of analysis were less than 0.9%. The recoveries of quantified compounds ranged from 98.63 to 103.85%. The developed UPLC method was found to be effective, convenient and sensitivity for quantitative analysis of seven compounds in H. cordata. This work could be provided a baseline source for quality control of H. cordata.

• 한국환경과학회지
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• 제28권10호
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• pp.851-861
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• 2019

In this study, we performed a sediment elution experiment to evaluate water quality in terms of phosphorus, as influenced by the dissolved oxygen consumed by sediments. Three separate model column treatments, namely, raw, calcined, and sonicated oyster shell powders, were used in this experiment. Essential phosphorus fractions were examined to verify their roles in nutrient release from sediment based on correlation analyses. When treated with calcined or sonicated oyster shell powder, the sediment-water interface became "less anaerobic," thereby producing conditions conducive to partial oxidation and activities of aerobic bacteria. Sediment Oxygen Demand (SOD) was found to be closely correlated with the growth of algae, which confirmed an intermittent input of organic biomass at the sediment surface. SOD was positively correlated with exchangeable and loosely adsorbed phosphorus and organic phosphorus, owing to the accumulation of unbound algal biomass-derived phosphates in sediment, whereas it was negatively correlated with ferric iron-bound phosphorus or calcium fluorapatite-bound phosphorus, which were present in the form of "insoluble" complexes, thereby facilitating the free migration of sulfate-reducing bacteria or limiting the release from complexes, depending on applied local conditions. PCR-denaturing gradient gel electrophoresis revealed that iron-reducing bacteria were the dominant species in control and non-calcined oyster shell columns, whereas certain sulfur-oxidizing bacteria were identified in the column treated with calcined oyster powder.

• Journal of Ginseng Research
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• 제37권4호
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• pp.457-467
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• 2013

A quick and simple method for simultaneous determination of the 30 ginsenosides (ginsenoside Ro, Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, 20(S)-Rg2, 20(R)-Rg2, 20(S)-Rg3, 20(R)-Rg3, 20(S)-Rh1, 20(S)-Rh2, 20(R)-Rh2, F1, F2, F4, Ra1, Rg6, Rh4, Rk3, Rg5, Rk1, Rb3, Rk2, Rh3, compound Y, compound K, and notoginsenoside R1) in Panax ginseng preparations was developed and validated by an ultra performance liquid chromatography photo diode array detector. The separation of the 30 ginsenosides was efficiently undertaken on the Acquity BEH C-18 column with gradient elution with phosphoric acids. Especially the chromatogram of the ginsenoside Ro was dramatically enhanced by adding phosphoric acid. Under optimized conditions, the detection limits were 0.4 to 1.7 mg/L and the calibration curves of the peak areas for the 30 ginsenosides were linear over three orders of magnitude with a correlation coefficients greater than 0.999. The accuracy of the method was tested by a recovery measurement of the spiked samples which yielded good results of 89% to 118%. From these overall results, the proposed method may be helpful in the development and quality of P. ginseng preparations because of its wide range of applications due to the simultaneous analysis of many kinds of ginsenosides.

• 한국식품영양학회지
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• 제32권2호
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• pp.148-154
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• 2019

The aim of this study was to select compounds for the standardization of fermented Kalopanax pictus Nakai (KP-F), to develop the analysis method using HPLC-PDA and to perform method validation. KP-F is a fermented powder developed to improve the original physiological activities and create a new functionality. Eleutheroside E, Acanthoside B, and Syringaresinol were selected as the standard compounds and developed our own method for simultaneous analysis. The analyte was isolated using C18 column with a gradient elution of 0.05 M phosphoric acid in water and methanol as the mobile phase at a flow rate of 1 mL/min and detected at 210 nm. As a result, all standard compounds showed good linearity with an $R^2$ (coefficient of correlation) of 1.000 and for the limit of detection range of $0.710{\sim}0.831{\mu}g/mL$, and the limit of quantification as $2.150{\sim}2.520{\mu}g/mL$. The precision was RSD (%) of less than 4.80%, while the accuracy was 4.70%>RSD (%) for the range 102.44~110.48%. In conclusion, the developed analysis method is suitable for the detection of Eleutheroside E, Acanthoside B, and Syringaresinol in KP-F.

• Mass Spectrometry Letters
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• 제10권1호
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• pp.18-26
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• 2019

We developed a bioanalytical method for simultaneous determination of nine NBOMe derivatives (25H-NBOMe, 25B-NBOMe, 25E-NBOMe, 25N-NBOMe, 25C-NBOH, 25I-NBOH, 25B-NBF, 25C-NBF, and 25I-NBF) in human plasma using liquid chromatography tandem mass spectrometry (LC-MS/MS). Human plasma samples were pre-treated using solid-phase extraction. Separation was achieved on a C18 column under gradient elution using a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Mass detection was performed in the positive ion mode using multiple reaction monitoring. The calibration range was 1-100 ng/mL for all quantitative analytes, with a correlation coefficient greater than 0.99. The intra- and inter-day precision and accuracy varied from 0.85 to 6.92% and from 90.19 to 108.69%, respectively. The recovery ranged from 86.36 to 118.52%, and the matrix effects ranged from 27.09 to 99.72%. The stability was acceptable in various conditions. The LC-MS/MS method was validated for linearity, accuracy, precision, matrix effects, recovery and stability in accordance with the FDA guidance. The proposed method is suitable for reliable and robust routine screening and analysis of nine NBOMe derivatives in forensic field.

• 생약학회지
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• 제51권4호
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• pp.291-296
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• 2020

Filipendula glaberrima (FG) is a plant endemic to South Korea. It is economically important as a food source and used as a medicine in treating ailments. Filipendula flowers are characterized by the presence of several polyphenolic constituents. The aim of this study is to determine the content of (+)-catechin in Filipendula glaberrima collected from different regions at different flowering stages. High-performance liquid chromatography with a gradient elution system (0.5% acetic acid in water : acetonitrile = 95 : 5 to 0 : 100 for 35 min) was used. A reverse-phase INNO column with UV detection at 278 nm was employed. The results revealed that F. glaberrima from Mt. Odae has the highest (+)-catechin content (10.600 mg/g). Furthermore, its content was the lowest in samples collected during the pre-flowering period and the highest at the early-flowering stage. This study provides a basis in establishing the optimal period and the best region for collecting F. glaberrima with maximized (+)-catechin yield.

• Mass Spectrometry Letters
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• 제12권1호
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• pp.1-10
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• 2021

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

• 분석과학
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• 제34권4호
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• pp.160-171
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• 2021

Synthetic azo dyes are used extensively in herbal medicines to render the medicines more visually attractive to consumers. This study developed and validated a rapid high-performance liquid chromatography (HPLC) method to determine whether synthetic colorants such as Tartrazine, Auramine O, Metanil yellow, Sunset yellow, and Orange II are used extensively in Typha orientalis. To increase the recovery of the synthetic dyes, this method employed containing 50 mM ammonium acetate in 70 % methanol at first extraction and 100 mM HCl in 70 % methanol at second extraction. Five synthetic pigments in Typha orientalis were separated by gradient elution with a mobile phase consisting of acetonitrile and 50 mM ammonium acetate in distilled water at ultra-violet (UV) detection 428 nm or 500 nm. Additionally, this study established the liquid chromatography tandem mass spectrometry (LC-MS/MS) method to confirm positive samples suspected by HPLC results. The HPLC-UV method had good linearity, indicating r²> 0.999. The recoveries of the samples spiked with three different concentration ranged from 73.8~91.5 %, and relative standard deviation values indicated 0.2~5.2 %. The established LC-MS/MS could successfully identify the synthetic pigments in herbal medicine samples. The study demonstrates that Typha orientalis adulterated by yellowish synthetic dyes can be successfully distinguished when using the HPLC-UV method.

• 분석과학
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• 제20권5호
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• pp.442-447
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• 2007

마늘(Allium sativum L.)의 특성은 organosulfur 화합물이다. 마늘에 포함된 diallyl disulfide(DADS)를 분석하기 위한, 간단하고 신속한 시료준비와 분석방법을 제시하였다. 모든 마늘시료들은 메탄올, 벤젠, 또는 테트라하이드로퓨란과 같은 용매로 추출하여 분석하였다. 실험결과에 의하면, 메탄올로 추출한 시료가 가장 우수하였다. 분석조건으로는 이동상은 메탄올과 물로 구성되고 기울기법을 적용하였다. 분말가루로 된 마늘 1 g에 0.61 mg DADS를 추출하였다. 기존 분석방법에 비해 우수하여 마늘관련 연구에 도움이 될 것이다.