• Title/Summary/Keyword: 액체크로마토그래프법

Search Result 6, Processing Time 0.02 seconds

Quality Evaluation of Herbal Prescription, Oc Chun San, Employing Simultaneous Determination of the Marker Compounds by HPLC (HPLC를 이용한 옥천산 중 갈근, 감초, 오미자 지표성분의 다성분 동시분석)

  • Yoo, Jeong-Lim;Jang, Dae-Sik;Kim, Jin-Sook
    • Korean Journal of Oriental Medicine
    • /
    • v.11 no.2
    • /
    • pp.167-178
    • /
    • 2005
  • As a part of the quality control of herbal prescriptions which has been used for diabetes and related diseases, a reversed-phase liquid chromatographic method was developed for the simultaneous quantification of the three marker compounds, puerarin (Puerariae Radix), glycyrrhizin (Glycyrrhizae Radix), schizandrin (Schizandrae Fructus) in Oc Chun San. The HPLC analysis method was validated for parameters such as linearity, Limits of Detection(LOD), quantification(LOQ), repeatability, stability and recovery.

  • PDF

Determination of Trace Aldehydes in Ambient Air by Liquid Chromatography (액체 크로마토그래프법에 의한 대기시료중 미량 알데히드류의 정량)

  • 이용근;정태우
    • Journal of Korean Society for Atmospheric Environment
    • /
    • v.11 no.4
    • /
    • pp.339-349
    • /
    • 1995
  • The purpose on this study is to optimize the chromatographic determination method of trace aldehydes in ambient air. Carbonyl compounds in urban air were trapped at $C_{18}$ DNPH-coated cartridges, and generated hydrazone derivatives were separated by HPLC and detected by UV-vis spectroscopic detector at 360nm. Formaldehyde and acetaldehyde compounds could be isolated from urban(Seoul) air with more than 95% collection efficiency. The analytical detection limits for formaldehyde and acetaldehyde are 0.06pp $b_{v}$, 0.08pp $b_{v}$ for 108 L air samples, respectively. The precision of this method are 3 .sim. 4%(RSD) for mutiple injection of hydrazone standards. Separation of seven dinitrophenylhydrazones could be achieved in appoximately 20 minutes operation time using $C_{18}$ column with apprepriate eluent. The method was applied to the analysis of aldehydes and ketone in Seoul ambient air. The 24-h ambient levels of formaldehyde, acetaldehyde reached up to 6 .sim. 14 and 3 .sim. 8ppbv, respectively. The daily average concentration ratio were 0.60 for acetaldehyde/formaldehyde.yde.

  • PDF

Determination of Terazocin in Human Plasma by Liquid Chromatography and Bioequivalence Study of Teratonin® Tablets (액체크로마토그래프법에 의한 사람 혈장 중 테라조신의 정량 및 테라토닌® 정의 생물학적 동등성)

  • Cho, Eun-Sook;Kang, Sung-Ha;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
    • /
    • v.32 no.2
    • /
    • pp.119-125
    • /
    • 2002
  • A rapid, selective and reproducible high-performance liquid chromatographic method has been developed for the determination of terazocin in human plasma. Terazocin plus the internal standard, prazocin hydrochloride, were extracted from alkalified plasma with tert-butylmethyl ether, back-extracted into 0.05% phosphoric acid. Fifty ${\mu}l-portions$ of extract were injected onto a octadecylsilane column and eluted with a mixture of acetonitrile, water and triethylamine (30 : 70 : 0.1 v/v, adjusted to pH 5.0 with dilute phosphoric acid) at a flow rate of 1.0 ml/min. The fluorescence intensity of column eluents was monitored at excitation wavelength of 250 nm and emission wavelength of 370 nm. No interference peaks were observed. The practical limit of quantitation was 5 ng/ml for terazocin. The average intraday and interday coefficients of variation were 4.15 and 3.54%, respectively. Also intraday and interday precisions over the range $5{\sim}60\;ng/ml$ were $0.49{\sim}2.92\;and\;0.38{\sim}5.12%$, respectively. The bioequivalence of two terazosin tablets, the $Hytrine^{\circledR}$ (Il Yang Pharmaceutical Co., Ltd.) and the $Teratonin^{\circledR}$ (Sam-A Pharmaceutical Co., Ltd.), was evaluated according to the guideline of Korea Food and Drug Administration (KFDA). Sixteen healthy male volunteers $(24.6{\pm}2.0\;years\;old)$ were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After one tablet containing 2 mg of terazosin was orally administered, blood was taken at predetermined time intervals and the concentration of terazosin in plasma was determined with a HPLC method using spectrofluorometric detector. AUC was calculated by the linear trapezoidal method. $C_{max}\;and\;T_{max}$ were compiled from the plasma drug concentration-time data. Analysis of variance (ANOVA) was utilized for the statistical analysis of the parameters. The results showed that the differences in $AUC_t,\;C_{max}\;and\;T_{max}$ between the two preparations were 0.21 %, 5.53% and 8.82%, respectively. The powers $(1-{\beta})\;for\;AUC_t,\;C_{max}\;and\;T_{max}$ were >99%, 97.49%, and 33.26%, respectively. Minimum detectable differences $({\Delta},\;%)\;at\;{\alpha}=0.1\;and\;1-{\beta}=0.8$ and the 90% confidence intervals were all less than ${\pm}20%$ except for $T_{max}.\;AUC_t\;and\;C_{max}$ met the criteria of KDFA for bioequivalence, indicating that $Teratonin^{circledR}$ tablets are bioequivalent to $Hytrine^{circledR}$ tablets.

Determination of Formaldehyde in Cosmetics Using a Convenient DNPH Derivatization Procedure Followed by HPLC Analysis (간편한 DNPH 유도체화 HPLC 분석법을 이용한 화장품 중 포름알데하이드 분석)

  • Choi, Jongkeun
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.42 no.1
    • /
    • pp.65-73
    • /
    • 2016
  • Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

Simultaneous Determination of 8 Preservatives (6 Parabens, 2-Phenoxyethanol, and Chlorphenesin) in Cosmetics by $UPLC^{TM}$ ($UPLC^{TM}$를 이용한 화장품 중 보존제 8종(파라벤 6종, 페녹시에탄올, 클로페네신)의 동시분석)

  • Park, Jeong-Eun;Lee, So-Mi;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.33 no.4
    • /
    • pp.263-267
    • /
    • 2007
  • Parabens are used in nearly all types of cosmetics and toiletries because they are formulated well and have broad spectrum of activity, interness, low costs and excellent chemical stability in relation to pH. 2-phenoxyethanol and chlorphenesin are common preservatives which are usually used in combination with parabens in cosmetics. Toxicity of parabens is generally low but application of parabens to damaged or broken skin has resulted in sensitization. Moreover, the possibility of their estrogenic potential, anesthetic effects and reproductive toxicity has been reported. Consequently there are some regulations in use of parabens. And the maximum permitted concentrations of chlorphenesin and 2-phenoxyethanol in cosmetic products are authorized by the same reasons. So it is important to control and estimate the amount of parabens in products. In this article, we proposed a valid method for the simultaneous determination of 8 preservatives including parabens in a short time using ultra performance liquid $chromatography^{TM}\;(UPLC^{TM})$. Separation of eight components was achieved in less than 10 min and resolutions were reasonable (USP resolution ${\geqq}\;2$). And limit of detection and quantification were evaluated. The method was suitably validated for specificity, linearity, precision (repeatability, intermediate precision) and accuracy for assay (recovery) based on International conference on harmonisation (ICH) guideline. The method was applicable to analysis of preservatives in cosmetic products.