• Title/Summary/Keyword: Analytical Chromatography

Search Result 1,121, Processing Time 0.028 seconds

Analytical Method for Methylxanthin, Catechin, and Theaflavin Determinations in Korean Commercial Teas by HPLC (차에 함유된 methylxanthin류, catechin류 및 theaflavin류의 HPLC에 의한 동시분석법)

  • Kim, Soo-Yeun;Kozukue, Nobuyuki;Han, Jae-Sook;Lee, Kap-Rang
    • Korean Journal of Food Science and Technology
    • /
    • v.38 no.1
    • /
    • pp.5-9
    • /
    • 2006
  • Method for separation and quantification of methylxanthins, catechins, and theaflavins in Korean commercial teas (green, oolong, and black teas) was developed using reversed phase high-performance liquid chromatography (HPLC). After extraction with hot water, tea compounds were separated on Inertsil ODS-3v $(5\;{\mu}m)$ column, eluted with gradient of 7% acetonitrile and 93% of 20 mM phosphate buffer mixture for 7 min. Column effluent was monitored at 270 nm. This technique was effective for analyses of m methylxanthins, catechins, and theaflavins in teas and biological samples. In green and oolong teas, two kinds of methylxanthins and 7 of catechins were identified, whereas 4 theaflavins were only identified in black tea. Among seven catechins in green and oolong teas, EGCG showed highest amount, whereas ECG was highest in black tea. (theaflavins were found only in black teas) In all teas, theobromine content was lower than that of caffeine.

Assessment on the Extraction Efficiency of Explosive Compounds in Soil for Improving the Working Draft of International Standard (국제표준(안) 개선을 위한 토양 중 화약물질 추출 효율성 평가)

  • Lee, Goon-Taek;Jung, In-Ho;Kim, Bo-Hyun;Kim, Dong-Wook
    • Journal of Soil and Groundwater Environment
    • /
    • v.17 no.1
    • /
    • pp.42-46
    • /
    • 2012
  • The ISO document of ISO/TC/190/SC3/WG11/N11 is a working draft of international standard (WD) dealing with analytical method for the determination of explosives and related compounds using high performance liquid chromatography. The scope of this WD covers the storage of samples, preparing test portion, extraction and instrumentation. The main purpose of this study was to improve the extraction conditions which were already adopted in the WD. For this purpose, mechanical shaking method could be corresponded up to 18 hours of ultrasonic bath extraction in the WD was tested. Methanol was also tested with the intention of being added as an extracting solvent other than acetonitrile in the WD. According to the results, 16 hours of mechanical shaking method showed statistically the same effectiveness as that of 18 hours of ultrasonic bath extraction. In case of extracting solvent, methanol also showed statistically the same extraction capability as acetonitrile for DNB, TNT, 2-A-DNT and 2,4-DNT. However, the recovery rate of TNB with methanol extraction was 40% higher than that of acetonitrile extraction. Through adding mechanical shaking method into committee draft (cf. the next stage draft of the WD during the process for making international standard), ISO standard of analyzing explosives and related compounds in soil would become more useful in dealing with huge number of field samples in the laboratory. In other aspect, adopting methanol as an alternative extracting solvent would be very effective in the terms of exchangeability with GC-ECD/MS method which is being developed by German experts.

Isolation and Quantitative Analysis of Schisandrin, Gomisin A and Gomisin M2 From Schisandra chinensis (오미자로부터 Schisandrin, Gomisin A, Gomisin M2의 분리 및 함량 분석)

  • Kim, Yeong-Eun;Kim, Eun-Nam;Jeong, Gil-Saeng
    • Korean Journal of Pharmacognosy
    • /
    • v.50 no.2
    • /
    • pp.148-153
    • /
    • 2019
  • The lignan compound of Schisandra chinensis Baill. (Schizandraceae) has been reported to have a variety of biological activities such as liver protection, neuroprotection, anti-oxidant and anti-diabetes. In this study, we investigated a quantitative analytical method for schisandrin, gomisin A and gomisin $M_2$ isolated from S. chinensis by high-performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). The isolated compounds were identified by the analysis of 1H- and 13C-NMR spectroscopic data. The results showed that calibration curves of three compounds indicated great linearity with a correlation coefficient ($R^2$) of schisandrin 0.9983, gomisin A 0.9982 and gomisin $M_2$ 0.9986. The limits of detection (LOD) of schisandrin, gomisin A and gomisin $M_2$ were 0.14, 0.07 and $0.05{\mu}g/ml$ and the limits of quantification (LOQ) were 0.42, 0.22 and $0.14{\mu}g/ml$. Intra-day and inter-day precisions of schisandrin were 0.40~1.44%, 0.07~1.02% gomsin A were 0.22~0.52%, 0.10~0.63%, gomisin $M_2$ were 0.40~0.99%, 0.81~2.88%. In result, contents of schisandrin, gomisin A and gomisin $M_2$ in ethanol extract of S. chinensis were $25.95{\pm}0.15$, $2.51{\pm}0.02$ and $2.17{\pm}0.07mg/g$.

Optimization of 1D 1H Quantitative NMR (Nuclear Magnetic Resonance) Conditions for Polar Metabolites in Meat

  • Kim, Hyun Cheol;Ko, Yoon-Joo;Kim, Minsu;Choe, Juhui;Yong, Hae In;Jo, Cheorun
    • Food Science of Animal Resources
    • /
    • v.39 no.1
    • /
    • pp.1-12
    • /
    • 2019
  • The objective of this study was to establish an optimized 1D $^1H$ quantitative nuclear magnetic resonance (qNMR) analytical method for analyzing polar metabolites in meat. Three extraction solutions [0.6 M perchloric acid, 10 mM phosphate buffer, water/methanol (1:1)], three reconstitution buffers [20 mM 3-morpholinopropane-1-sulfonic acid, 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid, phosphate buffer], and two pulse programs (zg30, noesypr1d) were evaluated. Extraction with 0.6 M perchloric acid and 20 mM phosphate resulted in a stable baseline and no additional overlap for quantifying polar metabolites in chicken breast. In qNMR analysis, zg30 pulse program (without water-suppression) showed smaller relative standard deviation (RSD) and faster running time than noesypr1d (water-suppression). High-performance liquid chromatography was compared with qNMR analyses to validate accuracy. The zg30 pulse program showed good accuracy and lower RSD. The optimized qNMR method was able to apply for beef and pork samples. Thus, an optimized 1D $^1H$ qNMR method for meat metabolomics was established.

Analysis of the Marker Compounds in Sagunja-tang by LC-ESI-MS (LC-ESI-MS에 의한 사군자탕의 지표성분 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
    • /
    • v.50 no.1
    • /
    • pp.65-71
    • /
    • 2019
  • One of the oriental medicine prescriptions, Sagunja-tang consists of four herbal medicines (Ginseng Radix, Poria Sclerotium, Atractylodis Rhizoma Alba, and Glycyrrhiziae Radix et Rhizoma) and has been used as a medicine to enhance tonify the function of spleen and stomach in Korea. In this study, we conducted simultaneous analysis of the 9 marker components, liquiritin apioside, liquiritin, ginsenoside Rg1, liquiritigenin, ginsenoside Rb1, glycyrrhizin, atractylenolide III, atractylenolide II, and atractylenolide I in Sagunja-tang using a liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS/MS). Marker compounds were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, 1.7 mm) and the column was maintained at $45^{\circ}C$. The mobile phase consists of 0.1% (v/v) aqueous formic acid and acetonitrile with gradient condition. The LC-MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS system with multiple reaction monitoring (MRM) method in the positive and negative modes. The calibration curves of the nine marker components showed good linearity with coefficient of determination ${\geq}0.9984$ within tested range. The limits of detection and limits of quantification values were 0.27-2.42 ng/mL and 0.81-7.27 ng/mL, respectively. The concentrations of tested 9 analytes in the lyophilized Sagunja-tang sample using the established LC-ESI-MS/MS MRM method were detected up to 16.593 mg/g. These results can be useful as a basic data for the quality control of an oriental medicine prescriptions.

The contents of β-carotene and cholesterol in selected types of agricultural and processed foods in Korea

  • Duan, Bei Bei;Shin, Jung-Ah;Lee, Ki-Teak
    • Korean Journal of Agricultural Science
    • /
    • v.46 no.2
    • /
    • pp.315-322
    • /
    • 2019
  • In this study, the contents of ${\beta}$-carotene and cholesterol were evaluated in various types of agricultural and processed foods (vegetables, legume products, dairy products, and eggs). Certified reference material (CRM) with an assigned value was used for the validation of the ${\beta}$-carotene and cholesterol analytical methods. High recoveries (accuracy) of ${\beta}$-carotene (96%) and cholesterol (97%) were obtained from the quantitative analysis of the CRM, with a relative standard deviation (%) of 1.86 and 3.35% for the ${\beta}$-carotene and cholesterol, respectively. Vegetables contained relatively high concentrations of ${\beta}$-carotene (raw Toona sinensis, $1650.97{\mu}g/100g$, a raw small onion, $879.09{\mu}g/100g$, and a raw lettuce stem, $591.89{\mu}g/100g$). The ${\beta}$-carotene values in dried chickpeas ($22.94{\mu}g/100g$) and dried brown lentils ($21.98{\mu}g/100g$) were similar. The highest ${\beta}$-carotene value among the analyzed dairy products was found in banana milk ($234.21{\mu}g/100g$) while other flavored products (strawberry milk and chocolate milk) did not contain any ${\beta}$-carotene. Furthermore, ${\beta}$-carotene was not detected in goat milk and high calcium milk in this study. With regard to cholesterol among the analyzed samples, the highest cholesterol value was found in egg yolk (629.30 mg/100 g), and cooking methods (boiling and frying) had little effect on the cholesterol levels of eggs. In addition, the cholesterol content in vanilla ice cream was 28.77 mg/100 g which was the highest value among the analyzed dairy products.

HPLC/DAD Method Validation of 6-Hydroxyluteolin 7-O-Glucoside Analysis from Salvia plebeia (곰보배추에 함유된 6-Hydroxyluteolin 7-O-Glucoside 분석을 위한 HPLC/DAD 분석법 밸리데이션)

  • Lee, Hak-Dong;Paje, Leo Adrianne;Choi, Jungwon;Kim, Juree;Yu, A Ram;Bae, Min-Jung;Lee, Sanghyun
    • Korean Journal of Pharmacognosy
    • /
    • v.52 no.3
    • /
    • pp.186-191
    • /
    • 2021
  • We developed a method to identify and quantify 6-hydroxyluteolin 7-O-glucoside in the powder of Salvia plebeia (PS) using high-performance liquid chromatography coupled with diode array detector (HPLC/DAD) and equipped with reverse-phase INNO C18 column. The analytical method was optimized and validated using novel parameters. The obtained values for the limits of detection and quantification were 3.60 and 10.90 ㎍/mL, respectively. Calibration curve showed good linearity in the concentration range tested (0.00625-0.1 mg/mL, r2 = 1.0000), high accuracy (96.2-101.4%), and precision values (RSD ≤ 0.27%). Our analysis support the use of our method for accurately identifying and quantifying 6-hydroxyluteolin 7-O-glucoside from PS in routine analyses and large-scale extraction processes for content determination.

Quality Control of Majoon-e-Nisyan and its Acute Oral Toxicity Study in Experimental Rats

  • Shaikh, Masud;Husain, Gulam M.;Naikodi, Mohammed Abdul Rasheed;Kazmi, Munawwar H.;Viquar, Uzma
    • CELLMED
    • /
    • v.11 no.1
    • /
    • pp.2.1-2.8
    • /
    • 2021
  • The clinical condition Amnesia causes difficulty in learning new information and the inability to recall past events. It is primarily concerned with recent memory loss. Majoon-e-Nisyan (MJN) is a polyherbal Unani formulation, present in a semi-solid form. It is widely used potent drug of the Unani System of Medicine (USM) for treating Nisyan (amnesia). In the present study polyherbal Unani formulation, MJN has been studied for its quality control and acute toxicity. Standardization (quality control) of drugs deals with drug identity, drug quality and purity determination. Standardization of MJN had been done as per the Unani pharmacopoeial parameters approved by World Health Organization (WHO) - Pharmacognostical parameters, Physico-chemical parameters, high-performance thin-layer chromatography (HPTLC), microbial load, aflatoxin, and heavy metals. Solvents and chemicals used in the study were of analytical grade and used instrument were calibrated. By conducting an acute oral toxicity study in rats, the safety of MJN was assessed. The limit test method of OECD guideline 425 was followed in the study. Results of standardization and standard operating procedures (SOPs) for preparation of MJN may serve as the standard reference in the future. The data generated in the study for the quality control of MJN proved the quality of formulation and shows that MJN is not toxic in rats following acute dosing up to 2000 mg/kg bw. The data obtained in the paper for MJN may be used as a standard guideline for preparation of the formulation which can save time, cost, and resources for future research endeavours.

Content Comparative Analysis and Classification for Piniellia ternate, P. pedatisecta and Typhonium flagelliforme by HPLC-PDA analysis (HPLC-PDA를 이용한 반하, 호장남성, 수반하의 분류 및 함량분석)

  • Jo, Ji Eun;Lee, A Yeong;Kim, Hyo Seon;Moon, Byeong Cheol;Choi, Goya;Ji, Yunui;Kim, Ho Kyoung
    • The Korea Journal of Herbology
    • /
    • v.28 no.5
    • /
    • pp.95-101
    • /
    • 2013
  • Objectives : A quantitative method using high performance liquid chromatography with a photodiode array detector(HPLC-PDA) was established for the quantitative analysis of the four main compound and pattern analysis to classification Piiellia ternate, P. pedatisecta and Typhonium flagelliforme. Methods : The analytical procedure for the determination of P. ternata, together with the known main compounds uracil, uridine, guanosine and adenosine was established. Optimum HPLC-PDA separation of these P. ternata was possible on Luna C18(2) column material, using water and acetonitrile as mobile phase. The method was validated according to regulatory guidelines. In addition, this assay method were analyzed for the content of four main compound in P. ternata, P. pedatisecta and T. flagelliforme and by data obtained from the HPLC-PDA analysis was performed principal component analysis(PCA). Results : Validation results indicated that the HPLC method is well suited for the determination of the roots of P. ternata with a good linearity ($r^2$ > 0.999), precision and recovery rates. Analysis of HPLC-PDA, the average content of uracil, uridine, guanosine and adenosine was significantly higher in P. ternate>P. pedatisecta> T. flagelliforme order. The application of PCA to main compound data by HPLC-PDA permitted the effective discrimination among the three species. Conclusions : Analysis of both HPLC-PDA and PCA confirmed the fact that four main compound and pattern profiles of P. ternata, P. pedatisecta and T. flagelliforme were different from each other.

Quantitative analysis of the marker compounds in the decoctions of Coptis chinensis-Scutellaria baicalensis at different proportion produced by 'Mixed decoction' and 'Single decoction mixture' (배합 비율에 따른 황련과 황금의 혼합 전탕액 및 개별 전탕 혼합액 내 성분 함량 분석)

  • Kim, Han-Young;Kim, Jung-Hoon
    • The Korea Journal of Herbology
    • /
    • v.35 no.3
    • /
    • pp.33-45
    • /
    • 2020
  • Objective : The present study aimed to evaluate the change of the content of 7 active components in decoctions produced by various proportional pairs of Coptis chinensis Franch and Scutellaria baicalensis Georgi in 'Mixed decoction (MD)' and 'Single decoction mixture (SDM)'. Methods : The samples of MDs were prepared by decocting C. chinensis : S. baicalensis with the ratios of 10 g:10 g, 10 g:20 g, and 20 g:10 g. Those of SDMs were prepared by blending each single decoction from C. chinensis and S. Baicalensis with the ratios of 1:1, 1:2, and 2:1. The samples were evaluated by high-performance liquid chromatography with statistical analyses. Results : The analytical methods, which were optimized and validated, were reliably applied to present research. The content of all components in both MDs and SDMs at C. chinensis : S. baicalensis = 1:1 ratio were reduced compared with single herb decoction. The components from each compositional herb in MDs were proportionally increased with the ratio of original herb increased, but inversely proportional to paired herb. The contents of components in MDs were significantly lower than those in SDMs at all ratios, except for high content of baicalin at C. chinensis : S. baicalensis = 2:1. Conclusion : It was concluded that MDs and SDMs as well as the proportions of herbs could affect the contents of the components from original herbal medicines. These results provide the information for the quality control of herbal medicine combined C. chinensis with S. baicalensis.