• Archives of Pharmacal Research
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• 제13권2호
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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.

• 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.

• 약학회지
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• 제37권1호
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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.

• Journal of Pharmaceutical Investigation
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• 제23권3호
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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.

• 분석과학
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• 제8권2호
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• pp.161-166
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• 1995

이온쌍 액체크로마토그래피(IP-HPLC)에 의해 마주송이풀 중 acteoside를 분리 정량하였다. 시료를 메탄올 40mL로서 4시간 추출하였다. 추출물에 대한 분리, 정제를 Sep-Pak $C_{18}$ catridge와 메탄올-물(메탄을 50%, 물 50%, 인산 완충용액 pH=8.0)을 사용하였다. HPLC 분리조건은 poly(styrene-divinylbezene) PRP-1 역상컬럼($15cm{\times}4.6mm$ i. d., $5.0{\mu}m$)과 이동상으로 $5.0{\times}10^{-3}M$ tetrabutylammonium bromide가 포함된 메탄올-물(메탄을 60%, 물 40%, 인산 완충용액 pH=8.2)을 사용하였다. 이와 같은 조건으로 강원도 평창군 일대에서 채집한 마주송이풀 중에 함유된 acteoside를 분리 정량한 결과 그 함량 범위가 0.062~0.076%였다.

• 대한화학회지
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• 제42권4호
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• pp.416-421
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• 1998

귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피(RPIP-HPLC)용리 거동에서 이온쌍 시약의 농도와 리간드 종류 효과를 연구하였다. 귀금속 이온 분석의 선택성은 사용한 티아크라운에테르의 고리를 구성하는 원자들의 수가 작을수록 좋았고, 귀금속-티아크라운에테르 착물의 용리 메카니즘은 이동상 중 이온쌍 시약인 도데실술폰산나트륨염(SDS)의 농도가 10 mM 이하일 경우 이온쌍 형성 메카니즘으로, 10 mM 이상일 경우 미쎌 형성 메카니즘으로 설명되었다. 결론적으로 몇 가지 귀금속-티아크라운에테르 착물들을 최적 조건에서 성공적으로 분리하였고, 흑백사진 정착액 중 Ag(Ⅰ) 이온 분리와 정량에 유용함을 증명하였다.

• 분석과학
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• 제15권3호
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• pp.190-195
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• 2002

본 연구에서는 ion-pair reversed-phase high performance liquid chromatography (IP-RP-HPLC)방식을 이용한 denaturing high performance liquid chromatography (DHPLC)방법을 사용하여 기관지 천식을 조절하는 ${\beta}_2$-교감신경수용체 유전자의 돌연변이를 검출하였다. 50명의 천식 환자의 혈액에서 genomic DNA를 추출하여 중합효소연쇄반응 (polymerase chain reaction, PCR)을 이용해 증폭하고, 그 산물을 DHPLC로 분석한 결과, 50개의 시료 가운데 15개 (30%)의 돌연변이를 검출하였다. 최종적으로 유전자 염기서열결정법을 통해 DHPLC의 돌연변이 검출률이 정확함을 확인하였다.

• 한국응용과학기술학회지
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• 제22권4호
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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.

• KSBB Journal
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• 제25권5호
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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.

• 분석과학
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• 제10권5호
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• pp.343-349
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• 1997

역상 이온쌍 고성능액체크로마토그래피(RP-IPC)에 의한 살균제 농약 kasugamycin(5-amino-2-methy-6-(2,3,4,5,6-pentahydroxy cyclohexyloxy) tetrahydropyran-3-yl-amino-${\alpha}$-iminoacetic acid)의 정량분석법을 확립하였다. Ksugamycin의 정량분석법을 확립하기 위해 RP-IPC에서 organic modifier의 농도, 용리액의 pH 및 상대이온(counter ion)의 종류와 농도에 의한 시료의 머무름 거동에 대한 영향을 조사 검토하였다. 확립된 최적 변수를 바탕으로 개발된 이 분석법은 kasugamycin의 품질관리에 활용할 수 있음을 확인하였다.