• Title/Summary/Keyword: ion-pair HPLC

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Determination of Total Glycyrrhetic Acid in Glycyrrhizae Radix by Second Derivative UV Spectrometry

  • Song, Seung-Bae;Choi, Jung-Kap;Yoo, Gyurng-Soo
    • Archives of Pharmacal Research
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    • v.13 no.2
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    • pp.174-179
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    • 1990
  • Second derivative (D2) spectrometry using ion-pair extraction technique was development for the determination of total glycyrrhetic acid (GA) in Glycyrrhizae Radix, Glycyr-rhizin (G) obtained from Glycyrrhizae Radix was hydrolyzed into GA in 2 N-HCI and methanol (1:1) and extracted from aqueous phase in the form of an ion-pair complex with tetrapentylammonium bromide (TPA) as a counter ion. Maximum D2 amplitude (Z value) was obtained when 1000-fold or greater molar ratio of TPA was used at pH 11. Reaction an effective extraction solvent of the ion-pair complex. The linearity of standard curve of ion-pair GA was obtained in the range of 4.120 $\mu$g/ml as GA. Assayed contents of GA in dry powder by D2 UV spectrometry and HPLC method were 5.31 $\pm$ 0.04% and 5.20 $\pm$ 0.008%, respectively.

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

  • Phi, Taek-San;Cho, Young;Sok, Dae-Eun;Cha, Seung-Hee;Chung, Yun-Su
    • Journal of Pharmaceutical Investigation
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    • v.21 no.3
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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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Microanalysis of Pancuronium Bromide in Urine and Blood by HPLC (HPLC를 이용한 뇨 및 혈액중의 Pancuronium Bromide의 미량분석)

  • 김박광;김양숙;박성배;이종숙;정규혁;김경님
    • YAKHAK HOEJI
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    • v.37 no.1
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    • pp.30-35
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    • 1993
  • HPLC/fluorescence detection method for the analysis of pancuronium bromide in biological fluids was developed. The method depends on the formation of insoluble red complex between pancuronium bromide and rose bengal in aqueous layer. This complex is quantitatively extracted from aqueous layer into chloroform layer. The complex is stable for 1 day in chloroform layer at room temperature. It was possible to analyze pancuronium bromide in the range of 0.05~0.5 $\mu\textrm{g}$/ml without the effect of co-prescribed drugs.

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High Performance Liquid Chromatographic Assay of Acebutolol and its Acetyl Metabolite in Plasma (혈장중 Acebutolol 및 그 Acetyl 대사체의 HPLC 분석)

  • Baek, Chai-Sun;Lin, Emil T.
    • Journal of Pharmaceutical Investigation
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    • v.23 no.3
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    • pp.133-137
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    • 1993
  • A high-performance liquid chromatographic assay using ion-pair reverse-phase system was developed for the separation of acebutolol and acebutolol acetyl metabolite in plasma. A ion-pair reversephase system consisting of an ODS-bonded silica column and a mixture of 20% $CH_3CN$, 0.1% $H_3PO_4$, 0.035 M heptanesulfonic acid and 0.005 M tetrabutylammonium hydrogen sulfate as the mobile phase were used. Triamterene was employed as an internal standard. Based on 0.2 ml of plasma, the detection limits were 10.4 ng/ml for acebutolol and 10.3 ng/ml of acebutolol acetyl metabolite at the signal-to-noise ratio of 3:1.

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Separation and Determination of Acteoside in Pedicularis resupinata var. oppositifolia by Ion Pair Liquid Chromatography (이온쌍 액체 크로마토그래피에 의한 마주송이풀 중의 Acteoside의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.161-166
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    • 1995
  • Determination of acteoside in Pedicularis resupinata var. oppositifolia has been studied using ion pair liquid chromatography. Sample was extracted with 40mL methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_{18}$ catridge and 8mL aqueous methanol eluent(methanol 50%, water 50%, phosphate buffer pH=8.0). Its determination was performed by means of IP-HPLC with a Hamilton PRP-1 polystyrene-divinylbenzene reversed phase column($15cm{\times}4.6mm$ i. d., $5{\mu}m$) and an aqueous methanol eluent(methanol 60%, water 40% phosphate buffer pH=8.2) containing of $5.0{\times}10^{-3}M$ tetrabutylammonium bromide. The established method was applied to the sample that was collected in area of Pyung Chang gun. As a result, its content ranges showed to be 0.062~0.076%.

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Reversed-Phase Ion-Pair High Performance Liquid Chromatographic Elution Behavior of Noble Metal-Thiacrown Ether Complexes (귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피 용리거동)

  • Chung, Yong Soon;Kim, Dong Won;Lee, Kang Woo;Kim, Chang Seok
    • Journal of the Korean Chemical Society
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    • v.42 no.4
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    • pp.416-421
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    • 1998
  • In the reversed-phase ion-pair high performance liquid chromatographic (RPIP-HPLC) elution behavior of noble metal-thiacrown ether complexes, the effects of the concentration of ion-pairing reagent and kind of ligands were studied. It was found that the less the number of atoms in the ring of the thiacrown ether molecule was, the larger the selectivity was, and the elution mechanism of the complexes was explained due to the formation of ion-pair when the concentration of sodium dodecyl sulfate (SDS) in mobile phase was lower than 10 mM and due to the formation of micelle when the SDS concentration was higher than 10 mM. As a conclusion, separations of the noble metal-thiacrown ether complexes in an optimum separation condition were accomplished successfully and the method was proved to be an useful one for the separation and determination of Ag (Ⅰ) ion in a black-white photographic fixing solution.

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Mutation Analysis in β2-Adrenergic Receptor Gene by Denaturing High Performance Liquid Chromatography (DHPLC) (DHPLC를 이용한 β2-교감신경수용체 유전자에서의 돌연변이 분석)

  • Park, Sang-Bum;Oh, Chung-Hun;Kim, Jong-Wan;Jang, Won-Cheoul
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.190-195
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    • 2002
  • We analysed mutation of ${\beta}_2$-adrenergic receptor gene that controls bronchial asthma by denaturing high performance liquid chromatography (DHPLC) according to ion-pair reversed-phase high performance liquid chromatography (IP-RP-HPLC). We extracted genomic DNA from 50 asthma patients, amplified DNA using PCR, and analysed PCR product by DHPLC. As a result, we obtained that mutation frequency was 15 (30%) among 50 cases. Consequently DHPLC mutation detection was confirmed that the result of direct sequencing was coincide exactly.

Resolution of Molecular Species of the Triacylglycerol Containing Petroselinic Acid $(cis-C_{18:1{\omega}12)$ by Silver Ion-HPLC

  • Joh, Yong-Goe;Kim, Seong-Jin
    • Journal of the Korean Applied Science and Technology
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    • v.22 no.4
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    • pp.339-348
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    • 2005
  • On the analysis of triacylglycerol (TG) from the kernels of Acanthopanax sessiliflorus by reversed phase-HPLC, it was separated into three main fractions of PN 44, 46 and 48, according to partition number (PN). On the contrary, it could be clearly classified into seven fractions of SMM, MMM, SMD, MMD, SDD, MDD and MDT by silver ion-HPLC by the number of double bond in the acyl chains of TG species. But resolution of so-called critical pairs of TG molecular species such as molecular pairs of $P_eLL$ $[C_{18:1{\omega}12}/(C_{18:2{\omega}6)2}]$ and OLL $[C_{18:1{\omega}9}/(C_{18:2{\omega}6)2}]$ and OOL $[(C_{18:1{\omega}9)2}/C_{18:2{\omega}6]$, and $P_eP_eL$ $[(C_{18:2{\omega}12)2}/C_{18:1{\omega}6]$ was not achieved $(P_e;$ petroselinic acid, L; linoleic acid, O; oleic acid). On the other hand, TG extracted from Aralia continentalis kernels were also fractionated into seven groups of SSM, SMM, MMM, SMD, MMD, SDD and MDD (S; saturated acid, M; monoenoic acid, D; dienoic acid) by silver ion-HPLC, although it's were classified into three groups of PN 44, 46 and 48 by reversed phase-HPLC. The fractions of SMM, MMM, MMD and MDD were divided into two subfractions, respectively; the fractions of SMM, MMM, MMD and MDD were resolved into the subfraction of $PP_e/P_e$ and POO (critical pairs from each other), that of $P_e/P_e/P_e$ and OOO, that of $P_e/P_e/L$ and OOL, and that of $P_e/L/L$ and OLL.

Simultaneous Determination of Tar Color Additives in Cold Syrups by Ion Pair-high Performance Liquid Chromatography (이온쌍-고성능 액체크로마토그래피에 의한 감기약 시럽에서 타르색소 첨가물의 동시분석)

  • Jin, Jing-Yu;Huang, Hu;Lee, Beom-Gyu;Lee, Won-Jae
    • KSBB Journal
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    • v.25 no.5
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    • pp.459-465
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    • 2010
  • A simple and efficient analytical method for the simultaneous determination of seven tar color additives was developed using ion pair high performance liquid chromatography. The conditions for HPLC analysis were as follows: column, ${\mu}$-Bondapak C18 (10 ${\mu}m$, 300 ${\times}$ 3.9 mm i.d.); gradient mobile phase, 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrile-methanol (65:25:10) as a mobile for fraction A and 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrilemethanol (40:50:10) as a mobile for fraction B; flow rate, 1.0 mL/ min; detection wavelength, 254/520/620 nm. We could attain to the detection limits as 0.01~0.05 ${\mu}$g/mL (254 nm) and 0.005~0.01 ${\mu}$g/mL (520 nm) for six red tar color additives, and 0.05 ${\mu}$g/mL (254 nm) and 0.002 ${\mu}$g/mL (620 nm) for Fast green FCF. This analytical method was applicable to determine the tar color additives contained in several commercial cold syrups.

Analysis of Kasugamycin in Pesticide Formulations by Reversed-Phase Ion Pair Liquid Chromatography (역상 이온쌍 액체크로마토그래피에 의한 농약 제품 중 Kasugamycin의 분석)

  • Kim, Taek-Jae;Kim, Kyong-Sun;Yoon, Chae-Hyuk;Joo, Jin-Bok;Kim, Chung-Hyo
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.343-349
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    • 1997
  • Analytical method using the reversed phase ion-pair chromatography (RP-IPC) for the determination of kasugamycin(5-amino-2-methyl-6-(2,3,4,5,6-pentahydroxy cyclohexyloxy)tetrahydropyran-3-yl-amino-${\alpha}$-imino acetic acid), pesticide as fungicide bactercide has been established. The retention behavior of kasugamycin in the RP-IPC was examined with respect to the effect of concentrations of organic modifiers, pH of eluent and types and concentrations of the counter ions as ion-pair reagent. This method developed by the optimum factors, can be used for the application of the quality control in the crude product and its formulation.

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