• 제목/요약/키워드: Simultaneous quantitative analysis

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Determination of Corticosteroids in Moisturizers by LC-MS/MS

  • Park, Sumin;Choi, Gye Young;Lee, Seon-Ah;Kim, Hyun Jeong;Yum, Hye Yung;Paeng, Ki-Jung
    • Mass Spectrometry Letters
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    • 제7권1호
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    • pp.26-29
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    • 2016
  • Simultaneous determination of three corticosteroids (clobetasol propionate, betamethasone dipropionate, fluticasone propionate) in moisturizers was performed by using liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS). Sample preparation was conducted by the liquid-liquid extraction (LLE). Moisturizers include emulsifying agent and it forms micelles. In order to improve the extraction efficiency of corticosteroids trapped in micelle, newly developed-optimized extraction conditions which can remove the matrix effect from moisturizers was applied with various pH conditions in LLE extraction stage of sample preparation. Thus, the addition of 10 μL of 1 M HCl into moisturizers sample before extraction could improve the extraction efficiency. For the quantitative analysis, SRM table that contained specific transition of all of target corticosteroids was created. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), limit of quantization (LOQ) and recovery. Over the 0.99 r2 value was obtained in calibration standard range. Effective accuracy and precision were also obtained. LODs were below 31 ng/mL and LOQs were estimated below 94 ng/mL for all corticosteroids tested.

피리도스티그민 정제의 함량 측정을 위한 HPLC 분석법 (Quantitative Analysis of Pyridostigmine Bromide in Tablets by HPLC)

  • 피택산;조영;석대은;차승희;정윤수
    • Journal of Pharmaceutical Investigation
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    • 제21권3호
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    • pp.171-177
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    • 1991
  • A reverse-phase, ion-pair high performance liquid chromatographic (HPLC) method for the simultaneous quantative determination of pyridostigmine and its hydrolytic product, 3-hydroxy-N-methylpyridinium (HMP), is descrihed, The assay of pyridostigmine and HMP was linear in the range of amount from 24 to 60 mg/tablet and from 2.4 to 12.0 mg/tablet, respectively, with coefficient of variation (C.V.) of 0.05-0.12% (n=7) and 0.25-0.52% (n=5), respectively, and applicable conveniently even in the case of the mixture of pyridostigmine and HMP. Meanwhile, the conventional UV method gave inaccurate results for the aged pyridostigmine tablets. In the extraction of pyridostigmine from tablets prior to be assayed by HPLC, methanol was found to be more effective than ethanol or distilled water. Multiple extraction (four times) with methanol resulted in the full recovery of pyridostigmine, whereas ethanol gave 95% recovery even after four times extraction. Based on these results. the present method would be very useful for the accurate determination of pyridostigmine in the aged pyridostigmine tablets.

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Development of analytical method of DMDM hydantoin, Sorbic acid, Phenoxy ethanol in Cosmetics

  • Kim, Young-Ok;Jang, Jung-Yun;Lee, Jeong-Pyo;Yang, Seong-Jun;Lee, Kyung-Shin;Yang, Won-Jun;Kim, Chong-Kap;Choi, Sang-Sook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.280.3-281
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    • 2003
  • A high-performance liquid chromatographic method for the simultaneous quantitative analysis of DMDM hydantoin, sorbic acid, phenoxy ethanol in cosmetics was studied by using a X-terra C18 column and 0.75mM KH2PO4 in 0.85% sulfuric acid and methanol mixture(7:3) at 214nm. Calibration curves were found to be linear in the 20-100$\mu\textrm{g}$/mL range (DMDM hydantoin), 50-250$\mu\textrm{g}$/mL range (sorbic acid) and 10-50$\mu\textrm{g}$/mL range (phenoxy ethanol). The result of recovery test were 96.6% - 104.2%. This HPLC method can be applied quality control of cosmetics.

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Quantitative Analysis of Bioactive Compounds in the Fruits of Crataegus pinnatifida by High-Performance Liquid Chromatography

  • Bae, Yoon-Ho;Cuong, To Dao;Lee, Jae-Hyun;Woo, Mi-Hee;Choi, Jae-Sue;Min, Byung-Sun
    • Natural Product Sciences
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    • 제18권2호
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    • pp.83-88
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    • 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.

UPLC-MS/MS를 이용한 산천목 중 10종 성분의 함량 분석 (Quantitative Analysis of the Ten Phytochmicals in Acer tegmentosum Maxim by UPLC-MS/MS)

  • 황윤환;이위;양혜진;마진열
    • 생약학회지
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    • 제49권1호
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    • pp.70-75
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    • 2018
  • Acer tegmentosum Maxim (ATM) has been used to treat hepatic disorders in traditional oriental medicine. However, there is little information about phytochemical constituents for quality control of ATM. In this study, we developed and established a simultaneous analytical method of the 10 marker compounds (three coumarins, 3 flavonoids, 1 lignan, 3 phenolics) in ATM using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS). Chromatographic separation of ten target analytes was achieved with a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$), using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. Identifications and quantitation of all analytes were performed using a Q-Exactive UPLC-MS/MS system. Correlation coefficients of the calibration curve for all analytes were ${\geq}0.9986$. The values of limits of detection and quantification of all analytes were 0.5-10.0 and 5.0-50.0 ng/mL, respectively. The established UPLC-MS/MS method successfully identified all target analytes in ATM, and the phytochemicals were 0.01-67.98 mg/g in its lyophilized water extract.

Rapid and Simultaneous Determination of Volatile Fatty Acids and Indoles in Pig Slurry and Dog Excrement by Solid-Phase Micro-Extraction Method with Gas Chromatography

  • Kim, Hyun-Jung;Yu, Mee-Seon;Yang, Sung-Bong
    • 한국환경과학회지
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    • 제23권10호
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    • pp.1693-1701
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    • 2014
  • A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. $50/30{\mu}m$ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to $0.15{\mu}gL$ for VFAs and from 0.12 to $0.28{\mu}gL$ for indoles and the correlations observed ($R^2$) were 0.975~1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

DEVELOPMENT OF ANALYYICAL METHOD OF DMDM HYDANTOIN, SORBIC ACID, PHENOXY ETHANOL IN COSMETICS

  • K. H. Son;Kim, Y. O.;J. Y. Jang;Lee, J. P.;S. J. Yang;Lee, K. S.;W. J. Yang;Kim, C. K.;Park, S. S.
    • 대한화장품학회:학술대회논문집
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    • 대한화장품학회 2003년도 IFSCC Conference Proceeding Book II
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    • pp.527-527
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    • 2003
  • A high-performance liquid chromatographic method for the simultaneous quantitative analysis of DMDM hydantoin, sorbic acid, phenoxy ethanol in cosmetics was studied by using a X-terra C$\sub$18/ column and 0.75mM KH$_2$PO$_4$ in 0.85% sulfuric acid and methanol mixture(7:3) at 214nm. Calibration curves were found to be linear in the 20-100 $\mu\textrm{g}$/mL range (DMDM hydantoin), 50-250 $\mu\textrm{g}$/mL range (sorbic acid) and 10-50 $\mu\textrm{g}$/mL range (phenoxy ethanol). The result of recovery test were 96.6% ∼ 104.2%. This HPLC method can be applied quality control of cosmetics.

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RP-HPLC를 이용한 백소엽(白蘇葉)과 자소엽(紫蘇葉)의 카페익산과 로즈마린산 분석 (Determination of Rosmarinic Acid and Caffeic Acid from Perilla frutescens var. japonica and var. acuta by Reversed-Phase HPLC)

  • 김병연;정지선;권하정;이제현;홍선표
    • 대한본초학회지
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    • 제23권3호
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    • pp.67-72
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    • 2008
  • Objectives : This study presents a high performance liquid chromatography methods for the quantitative and qualitative analysis of rosmarinic acid (RA) and caffeic acid (CA) in Perilla frutescens var. japonica and var. acuta. Methods : Chromatographic separation was performed using a mixture of methanol, water and formic acid (35 : 64.2 : 0.8) with a reversed-phase column (Gemini C18, 4.6 ${\times}$ 150 mm, 3 ${\mu}m$). The analyses were detected at UV (280 nm). Results : The samples were extracted with 50% EtOH under reflux for 1 h, and simultaneous determination for RA and CA in hyang-so-san and haeng-so-san was possible without interference peaks Conclusions : According the results, we developed a determination method for RA and CA in Perillae Folium. Owing to Perilla frutescens var. japonica and var. acuta did not show significant difference in contents of RA and CA, both Perilla frutescens could be available as herbal medicine.

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Do Long Term Savings Motives Foster Household Participation and Contribution to Savings Mechanisms in Rural Vietnam?

  • HA, Van Dung
    • The Journal of Asian Finance, Economics and Business
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    • 제6권2호
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    • pp.75-82
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    • 2019
  • The paper aims to investigate the impacts of long-term savings motives on fostering household participation and contribution to savings mechanisms in rural Vietnam. The paper is organized in five parts: introduction, data description, methodology, empirical results, and conclusion. The quantitative methodology is employed and three simultaneous estimation methods, including instrumental variable model, two-step model, and Heckman model are used to test these impacts as well as the robustness of results. In each model, the paper examines the impacts of independent factors on both household participation and household contribution to savings mechanisms. Two sets of independent variables: long-term savings motives (profit-making investment, accumulation for big expenditure, providing for old age, and cost of educations) and control variables (dependency rate, number of people in household, and household wealth) are in each model. A set of dataset of 2,314 households for analysis is obtained from household survey in rural Vietnam. Robust statistical findings indicate that profit-making investment emerged to be the strongest motive fostering household participation to savings mechanisms while other long-term savings motives have little or no impact on fostering household participation to savings mechanisms. In addition, education investment encourages household contribution to savings mechanisms in rural Vietnam.

Quantitative Analysis of Flavonoid Glycosides in Sophora japonica and Sophora flavescens by HPLC-DAD

  • Kim, Soo Sung;Park, SeonJu;Kim, Nanyoung;Kim, Seung Hyun
    • Natural Product Sciences
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    • 제27권4호
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    • pp.284-292
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    • 2021
  • Recently, a phytoestrogenic functional food has been developed using the fruits of Sophora japonica. Phytochemical investigation of fruits of S. japonica led to the isolation of eight flavonoid glycosides using various chromatographic techniques. The isolated compounds were identified as genistin (1), sophoricoside (2), genistein 7,4'-di-O-β-D-glucopyransoide (3), sophorabioside (4), genistein-7-O-β-D-glucopyranoside-4'-O-[(α-L-rhamnopyranosyl)-(1→2)-β-D-glucopyranoside] (5), sophoraflavonoloside (6), nicotiflorin (7) and kaempferol-3-O-α-L-rhamnopyranosyl-(1→6)-β-D-glucopyranosyl-(1→3)-β-D-glucopyranoside (8), respectively, by comparison of their spectroscopic data with those reported in the literature. In addition, a new HPLC-DAD method for simultaneous determination of the isolated compounds was developed to quantitate the contents of flavonoids in S. japonica and S. flavescens. The method was validated in terms of limit of detection, limit of quantitation, specificity, linearity, precision and accuracy. The validated method was successfully applied to determine eight flavonoids in two Sophora species. The contents of eight flavonoids varied according to the parts and species. Particularly, it was found that only the fruits of S. japonica contained sophoricoside, a phytoestrogenic isoflavone.