• Title/Summary/Keyword: HPLC analysis methods

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A Comparative Study on the Herbal Prescription and the Herbal Substance of Atractylodis Rhizoma Alba by HPLC analysis (한약제제 백출(白朮)과 한약재 백출에 대한 HPLC 분석 비교연구)

  • Cho, Hyun Joo;Jeon, Yoon Jae;Kim, Nam-Gil;Choi, Hyug-Yong
    • Herbal Formula Science
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    • v.24 no.2
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    • pp.71-79
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    • 2016
  • Objectives : To verify the equivalence between Atractylodis Rhizoma Alba herbal prescription(HP-ARA) and Atractylodis Rhizoma Alba herbal sub stance(HS-ARA). Methods : Safety tests by microbial regulation and heavy metal analysis (total heavy metal, Pb, As) and a stability test by long term shelf test for HP-ARA according to notification of the Ministry of Food and Drug Safety were carried out. Then, multi component profile of HP-ARA and HS -ARA were analyzed by HPLC. Results : The safety and stability of HP-ARA confirmed by several tests. Correlation coefficient of equivalence of HP-ARA and ARA-HS showed 0.992. Conclusion : Based on this result of equivalence between HP-ARA and HS-ARA, HP-ARA can substitute HS-ARA used to make herbal medicines (herbal decoction, pills and powder).

Evaluation on the Safety of ${\gamma}$-Irradiated Angelica gigas Nakai: Stability of Active Components and Safety in Genotoxicity Test (감마선 조사 당귀(Angelica gigas Nakai)의 유효성분 안정성 및 유전독성학적 안전성 연구)

  • 조성기;유영법
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.29 no.2
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    • pp.300-306
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    • 2000
  • In the present studies, we assessed the stability of active components and toxicological safety of irradiated Angelica gigas Nakai(Danggui). In order to confirm the stability of active components in the ${\gamma}$-irradiated roots of Danggui, the quantitative analysis of decursin and decursinol angelate of ${\gamma}$-irradiated sample was carried out by high performance liquid chromatographic (HPLC) methods using reverse phase columns and normal phase columns. From the root of Danggui, decursin and decursinol angelate were isolated by a silica gel column chromatography(toluene : ether (1 : 1), Hexane : EtOAc(15 : 1)). And then the structures were confirmed in the 1H and 13C-NMR analysis. The HPLC chromatograms of decursin and decursinol angelate in ${\gamma}$-irradiated Danggui were similar with those of non-irradiated sample. In the examination of in vitro genotoxicity of the water extract from ${\gamma}$-irradiated Danggui using Salmonella reversion assay(Ames test) and micronucleus test in Chinese hamster ovary (CHO) cells, mutagenicity was not exhibited in the two assays with or without metabolic activation. These resutls suggest that active components in the ${\gamma}$-irradiated Danggui should be stable and that the safety of ${\gamma}$-irradiated Danggui could be revealed in further test in vivo.

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Monitoring of Residual Veterinary Drugs in Incheon Fishery Products Distribution (인천 유통 수산물 중 잔류동물용의약품 조사)

  • Jang, Jin-Seob;Hur, Myong-Je;Kim, Meyong-Hee;Han, Young-Sun;Kwon, Sung-Hee;Yeo, Eun-Young;Hong, Seong-Hee;Kim, Ji-Sun;Lee, Seung-Ri
    • Journal of Environmental Health Sciences
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    • v.44 no.5
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    • pp.444-451
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    • 2018
  • Objectives: This study was carried out to provide safe seafood to the public through simultaneous analysis rapid inspections for residual veterinary drugs in 150 fishery products in 2016. Methods: Quinolones (9), Sulfonamides (14), Penicillins (2), Cephalosporins (3), Tetracyclines (4), Macrolides (4), Lincosamides (2), Pleuromutilin (1), Phenicols (4), benzylpyrimidines (2), Others (1) Malachite green (2), and Melamine (1) were analyzed for 49 species using by HPLC and HPLC-MSMS. Results: There were six unsuitable samples, five among fish and one for crustaceans. Within the standard detection were five fish. The antibiotics found were Quinolones (50%), Tetracyclines (33%) and Penicillins (17%). Conclusions: As a result of the experiment, there were six unsuitable samples, five for fish and one for crustaceans. The most prevalent antibiotics were Quinolones. The quinolone antibiotics are highly persistent in fish tissues, so they require more time than the withdrawal period for other common veterinary drugs. Careful attention is required when they are used in fish farms.

HPLC Analysis of Marker Substances in Taeumin Gamijowi-tang (태음인(太陰人) 가미조위탕(加味調胃湯)의 HPLC 분석)

  • Hwang, Young-Myung;Yu, Young-Beob;Kim, Jong-Youl;Koh, Byung-Hee;Lee, Eui-Ju
    • Journal of Sasang Constitutional Medicine
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    • v.18 no.1
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    • pp.147-154
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    • 2006
  • 1. Objectives This study was aimed to evaluate marker substances in Gamijowi-tang by high performance liquid chromatography(HPLC) 2. Methods The seperation was performed an AquasilC18(4.6X250mm)column by gradient elution with 0.1N H3PO4 in H2O - acetonitrile(0min 100:10,20min60:40, 40min 80:20, 60min 100:0) as the mobile phase at a flow-rate of 1.0 ml/min with detection at 190-800nm 3. Results Ephedrine and schizandrin were established as marker substances in Gamijowi-tang and its qualitative analysis was carried out. Analyzed was similarity of marker substances between in standard article and in Gamijowi-tang. The result of the analysis was that ephedrine and schizadrin showed 0.9999 of similarity, which meant they were really ephedrine and schizadrin. In addition, ephedrin content was 12.16mg, pseudoephedrine conrenr was 5.09mg, and schizandrin content was 26.6mg in 76g of Gamijowi-tang. 4. Conclusions Qualitative and quantitative analyses of ephedrine and schizandrin in Gamijowi-tang were conducted, and it was identified thar they could be used as marker substances in standardizing quality of Gamijowi-rang.

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Analytical Method for the Validation of Hispidulin as a Marker Compound for the Standardization of Salvia plebeia R. Br. Extracts as a Functional Ingredient (배암차즈기 추출물의 기능성원료 표준화를 위한 지표성분으로서 Hispidulin의 분석법 평가)

  • Jeon, Yoon Jung;Kwak, Hoyoung;Choi, Jong Gil;Lee, Je Hyuk;Choi, Soo Im
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.4
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    • pp.271-276
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    • 2016
  • Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

Expermental Studies of quantitative evaluation using HPLC and safety of Sweet Bee Venom (Sweet BV의 함량분석과 시술 부위별 LD50 관찰)

  • Chu, Ching-Seng;Park, Hee-Soo;Kim, Min-Ki;Cha, Bae-Chun;Lee, Eun;Kwon, Ki-Rok
    • Journal of Pharmacopuncture
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    • v.10 no.2 s.23
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    • pp.81-86
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    • 2007
  • Objectives : This study was conducted to carry out quantitative evaluation and safety of Sweet Bee Venom. Methods : Content analysis was done using HPLC, measurement of LD$^{50}$ was conducted intravenous, subcutaneous, and intramuscular injection to the ICR mice. Results : 1. According to HPLC analysis, removal of the enzymes containing phospholipase A2 was successfully rendered on Sweet Bee Venom. And analyzing melittin content, Sweet Bee Venom contained 12% more melittin than Bee Venom. 2. LD$^{50}$ of ICR mice with Sweet Bee Venom was more than 20mg/kg in subcutaneous injection and intravenous injection, between 15mg/kg and 20mg/kg in muscular injection. 3. LD$^{50}$ of ICR mice with Bee Venom was between 6 and 9mg/kg in subcutaneous injection and intravenous injection, and more than 9mg/kg in muscular injection. Conclusion : Above results indicate that Sweet Bee Venom was more safe than Bee Venom and the process of removing enzymes was well rendered in Sweet Bee Venom.

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
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    • v.42 no.1
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    • pp.65-73
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    • 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.

A Comparative Study of the Assay Methods Used to Quantify Fermentable Sugar in Makgeolli Sul-dut (막걸리 술덧의 발효성 당 분석방법 비교 연구)

  • Kim, Byong-Soo;Kim, Gye-Won;Shim, Jae-Yong
    • Korean Journal of Food Science and Technology
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    • v.48 no.1
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    • pp.48-53
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    • 2016
  • The objective of this study was to evaluate the accuracy and efficiency of different methods used for the fermentable sugar assay in the production of Makgeolli sul-dut. In the initial stage of fermentation, Ipguk treatment produced a higher alcohol content compared to the Nuruk treatment. However, the alcohol content was not significantly different between the two starters at the final stage of fermentation. Acidity in the Ipguk treatment was higher than that of Nuruk throughout the fermentation period. After analyzing the fermentable sugars using dinitrosalicylic acid (DNS), Fehling's method, refractometer, glucose kit, and high performance liquid chromatography (HPLC), it was confirmed that the HPLC method was the most accurate for fermentable sugar quantification. In both types of starters, DNS and Fehling's methods showed results comparable to HPLC in terms of fermentable sugar content, while the glucose kit and refractometer analyses showed relatively large discrepancies, indicating that the Fehling's method could also be effective for the analysis of fermentable sugars in the manufacture of Makgeolli.

Validation and Uncertainty Evaluation of an Optimized Analytical Method Using HPLC Applied to Canthaxanthin, a Food Colorant (식품 색소 Canthaxanthin의 HPLC 최적 분석법 확인 및 타당성과 측정불확도 평가)

  • Suh, Hee-Jae;Kim, Kyung-Su;Hong, Mi-Na;Lee, Chan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.3
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    • pp.342-351
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    • 2016
  • This study was carried out to develop an optimized analytical method using high-performance liquid chromatography (HPLC) applied to canthaxanthin, which is not yet designated as a food colorant in Korea, as well as to perform validation and uncertainty evaluation of this method. Official methods of AOAC, UK, and Japan with HPLC-UV detection were evaluated for the analysis of canthaxanthin by comparison of linearity, resolution, selectivity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, recovery, inter-laboratory tests, and uncertainty measurement. The calibration curves showed high linearity with an $R_2$ value of over 0.999 for canthaxanthin standard solutions in all three official methods. The official method of Japan exhibited the best results in terms of resolution and selectivity, including the lowest LOD and LOQ. The average coefficients of variation were calculated as less than five of three institutes with a precision value less than 1, accuracy near 100%, and recovery ratio between $100{\pm}10%$. The expanded uncertainty for canthaxanthin was estimated to be $39.5{\pm}5.29mg/kg$ (95% confidence level, k=2), and the uncertainty of measurement was 13.4%. In this study, official methods of canthaxanthin were compared and the validities verified. The results will be further applied to establish an authorized analytical method for canthaxanthin in Korea.

Effects of Herbal Medicine on Breastfeeding - Analysis of Marker Substances in Saenghwa-tang by HPLC and LC/MS/MS - (산모의 한약 복용이 모유에 미치는 영향 - HPLC와 LC/MS/MS를 이용한 생화탕 지표성분 분석 -)

  • Park, Ka-Young;Lee, Ah-Young;Ban, Ji-Hye;Park, Jung-Kyung;Lee, Eun-Hee
    • The Journal of Korean Obstetrics and Gynecology
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    • v.26 no.4
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    • pp.48-65
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    • 2013
  • Objectives: We took breast milk samples and analyzed them using HPLC and LC/MS/MS, to evaluate the effects of taking Saenghwa-tang during breastfeeding on breast milk. Methods: The study participants were 20 lactating women who admitted in Korean medical postpartum care center. Breast milks were collected from paticipants who have been administrated Saenghwa-tang for more than 3 days. We used HPLC and LC/MS/MS for the determinations of amygdalin, liquiritins, 6-gingerol, decursin and decursinol angelate in Saenghwa-tang. Results: 1. Participants' $Mean{\pm}S.D$ (standard deviation) of age is $31.05{\pm}1.96$, and 15 participants had normal delivery and 5 participants had cesarean delivery. 12 participants were primipara and 8 participants were multipara. $Mean{\pm}S.D$ of lactating date is $9.4{\pm}0.94$. 2. Using HPLC, we learned LOQ level peak that matches the peak retention time of standard components of Saenghwa-tang was not detected from 20 breast milk samples. 3. Using LC/MS/MS, decursin of Angelicae Gigantis Radix was detected from HMSP 02, HMSP 04, HMSP 06, HMSP 11, and the each concentrations are 16, 2, 64, 11 ppb. Liquiritin of Glycyrrhizae Radix was not detected from HMSP 13~HMSP 18. Conclusions: Data obtained by this approach shows that this method is reliable and suitable for determining the safety of taking Saenghwa-tang during breastfeeding.