• Title/Summary/Keyword: HPLC/DAD

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Establishment of Analytical Method for Carpropamid in Agricultural Commodities using HPLC-DAD/MS (HPLC-DAD/MS를 이용한 농산물 중 살균제 Carpropamid의 정밀 잔류분석법 확립)

  • Lee, Hyeri;Choi, Hoon;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.185-194
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    • 2015
  • This study was performed to establish a single residue analytical method for determining fungicide carpropamid residues in various agricultural commodities. Korean cabbage, apple, brown rice and green pepper were selected as representative crops. Samples were homogenized, extracted with acetone and purified by liquid-liquid partition and Florisil column chromatography. Carpropamid residues were analyzed at 220 nm with reversed phase HPLC equipped octylsilyl and octadecylsilyl column and confirmed using mass spectrometry. ILOQ (Instrumental limit of quantitation) of carpropamid was 2 ng and MLOQ (Method LOQ) was 0.02 mg/kg. Mean recoveries from four kinds of crop samples fortified at three levels (MLOQ, 10LOQ, 100LOQ) in triplicate were in the range of 84~112%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types.

Simultaneous Determination of Baicalin and Glycyrrhizin in Eul-Ja-Tang by HPLC/DAD

  • Lee, Mi-Kyeong;Lee, Ki-Yong;Kim, Seung-Hyun;Park, Jung-Hyun;Cho, Jung-Hee;Oh, Mi-Hyun;Baek, Ju-Hyun;Kim, Hyo-JIn;Kim, Young-Choong;Sung, Sang-Hyun
    • Natural Product Sciences
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    • v.14 no.3
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    • pp.147-151
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    • 2008
  • A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, baicalin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Eul-Ja-Tang (EJT). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/VIS detector (DAD) was used for the detection and the wavelength for quantification was set at 250 nm. The presence of baicalin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. Both baicalin and glycyrrhizin showed good linearity ($r^2$ > 0.999) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 5% and the limits of detection (LOD) were about 30 ng. The mean recovery of each compound was 99.5 - 101.2% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of baicalin and glycyrrhizin in three commercial products of EJT, which resulted in the difference in the contents of these compounds. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial EJT products.

Simultaneous Determination of Paeoniflorin and Glycyrrhizin in Sayuk-san by HPLC/DAD

  • Lee, Mi-Kyeong;Lee, Ki-Yong;Kim, Seung-Hyun;Jeon, Min-Ji;Cho, Jung-Hee;Oh, Mi-Hyun;Baek, Ju-Hyun;Kim, Hyo-Jin;Sung, Sang-Hyun
    • Journal of Pharmaceutical Investigation
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    • v.39 no.1
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    • pp.23-27
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    • 2009
  • A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, paeoniflorin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Sayuk-san (SYS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}150mm$) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of paeoniflorin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. All two compounds showed good linearity ($r^2$>0.996) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.3% and the limits of detection (LOD) were less than 55.7 ng. The mean recovery of each compound was $102.3{\sim}111.1%$ with R.S.D. values less than 4.6%. This method was successfully applied to the determination of contents of paeoniflorin and glycyrrhizin in three commercial products of SYS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial SYS products.

Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

Discrimination of biological and artificial nicotine in e-liquid

  • Hyoung-Joon Park;Heesung Moon;Min Kyoung Lee;Min Soo Kim;Seok Heo;Chang-Yong Yoon;Sunyoung Baek
    • Analytical Science and Technology
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    • v.36 no.1
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    • pp.22-31
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    • 2023
  • As the use of e-liquid cigarettes is rapidly increasing worldwide, it multiplies the potential risk undisclosed to the health of non- and smokers. To reduce the hazard, each country has its own set of regulations for controlling e-liquids. In Korea, the narrow definition of tobacco makes it difficult and have been steadily occurring tax evasion exploiting the difference in natural and artificial nicotine. Therefore, it is very important to distinguish source of nicotine for their regulation. To find biochemical discriminant markers, this study established analysis methods based on high-performance liquid chromatography coupled with diode array detector (HPLC-DAD) and high-performance liquid chromatography coupled with triple Quadrupole mass spectrometry (HPLC-MS/MS) for nicotine enantiomers and tobacco alkaloids targeted using the difference in pathways of nicotine biosynthesis and chemical synthesis. The method was validated by experimenting linearity (R2 > 0.999), recovery (80.99-108.41 %), accuracy (94.11-109.73 %) and precision (0.04-8.27 %). Then, the results for discrimination of the nicotine obtained from analysis of 65 commercial e-liquid products available in Korean market was evaluated. The method successfully applied to the e-liquids and one sample labelled 'synthetic nicotine' for tax exemption was found to contain a natural nicotine product. This method can be used to determine whether an e-liquid product uses natural or artificial nicotine and monitor non-taxable e-liquid products. The method is more scientific than the existing one, which relies only on field evidence.

Analysis of Nodakenetin from Samultangs Fermented by Lactose Bactera Strains (유산균 발효에 의한 사물탕들부터 노다케네틴의 분리 및 함량분석)

  • Kim, Dong-Seon;Roh, Joo-Hwan;Cho, Chang-Won;Ma, Jin-Yeul
    • The Korea Journal of Herbology
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    • v.27 no.1
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    • pp.35-39
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    • 2012
  • Objectives : The purpose of this study was to investigate the changes in the contents of constituents in Samultang and its fermentations with 10 species of lactic acid bacteria. Methods : Ten strains of lactic acid bacteria, Lactobacillus casei, L. acidophilus, L. casei, L. plantarum, L. amylophilus, L. curvatus, L. delbruekil subsp. lactis, L. casei, B. breve, and B. thermophilum, were used for the fermentation of Samultang. The increased and decreased constituents were identified using HPLC/DAD and various liquid chromatographic techniques, and the structure was elucidated using NMR and MS. These compounds were quantitatively analyzed using an HPLC/DAD system. Results : A remarkably increased component was identified to be nodakenetin and a decreased component was determined to be nodakenin. The fermentation of the ten lactic acid bacteria demonstrated that the decomposable rate of these two compounds in fermented Samultang were different. Samultang fermented by L. plantarum showed the most remarkable changes. Conclusion : Nodakenetin was identified as bioconversion component after fermentation and L. plantarum was discovered the best bacteria to increase the component.

Comparison of Hwangbek Dyeability for Cotton, Silk, and Wool from Different Tree Species and Origin (황백의 품종 및 산지에 따른 면, 견, 양모직물에 대한 염색성 비교)

  • Li, Longchun;Ahn, Cheunsoon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.38 no.1
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    • pp.110-122
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    • 2014
  • This study examined hwangbek dyeability for cotton, silk, and wool from different tree species and origin as well as their berberine and palmatine content. A total of 12 different hwangbek were examined, six purchased directly from different locations of China and six purchased from the Seoul Medicine Market. Hwangbek purchased from China were 3 Kwanhwangbek (Phellodendron amurense Rupr.) from Jilin, Liaoning, Heilongjiang and 3 Chunhwangbek (Phellodendron chinense Schneid.) from Sichuan, Yunnan, and Guangxi. Hwangbek purchased from the Seoul Medicine Market included 3 hwangbek that originated from Korea and 3 hwangbek imported from China. We extracted 2.5g of each hwangbek into 500mL of water for 60 min at $80^{\circ}C$. Dyeing was conducted using the IR dyeing machine for 30min at $55^{\circ}C$ using a 1:100 liquor ratio. Cotton was mordanted using tannic acid followed by potassium antimonyl tartrate trihydrate treatment before dyeing. Berberine and palmatine pigments in hwangbek were identified with the HPLC-DAD-MS instrument and the amount of pigment was quantified using an ion chromatogram. The results indicated that the K/S values of dyed fabrics were highly related to the amount of pigment in hwangbek used for dyeing.

Cognitive-Enhancing Effect of Dianthus superbus var. Longicalycinus on Scopolamine-Induced Memory Impairment in Mice

  • Weon, Jin Bae;Jung, Youn Sik;Ma, Choong Je
    • Biomolecules & Therapeutics
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    • v.24 no.3
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    • pp.298-304
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    • 2016
  • Dianthus superbus (D. superbus) is a traditional crude drug used for the treatment of urethritis, carbuncles and carcinomas. The objective of this study was to confirm the cognitive enhancing effect of D. superbus in memory impairment induced mice and to elucidate the possible potential mechanism. Effect of D. superbus on scopolamine induced memory impairment on mice was evaluated using the Morris water maze and passive avoidance tests. We also investigated acetylcholinesterase (AChE) activity and brain-derived neurotropic factor (BDNF) expression in scopolamine-induced mice. HPLC-DAD analysis was performed to identify active compounds in D. superbus. The results revealed that D. superbus attenuated the learning and memory impairment induced by scopolamine. D. superbus also inhibited AChE levels in the hippocampi of the scopolamine-injected mice. Moreover, D. superbus increased BDNF expression in the hippocampus. Eight compounds were identified using HPLC-DAD analysis. The content of 4-hydroxyphenyl acetic acid was higher than contents of other compounds. These results indicated that D. superbus improved memory functioning accompanied by inhibition of AChE and upregulation of BDNF, suggesting that D. superbus may be a useful therapeutic agent for the prevention or treatment of Alzheimer's disease.

A study on the analysis of artificial sweeteners in processed foods including emulsified foods by HPLC-DAD

  • Kim, Min-Hee;Lee, Do-Yeon;Ahn, Jang-Hyuk
    • Analytical Science and Technology
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    • v.33 no.5
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    • pp.209-214
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    • 2020
  • This study has been carried out to develop a standard method for quantifying of 3 permitted artificial sweeteners (including sodium saccharine, aspartame, acesulfame potassium) contained in foods by HPLC-DAD. A simple and rapid sample pretreatment method was used to remove fat and protein from the test solution with Carrez clearing regent precipitant know to be effective for protein and fat removal. The artificial sweeteners in the test solution purified through sample pretreatment were detected by high performance liquid chromatograph using a Reverse phase C18 column (5 ㎛, 4.6 × 250 mm). The simultaneous quantitative test of 3 kinds of artificial sweeteners can be effectively performed on the high fat emulsified foods containing a large amount of fat. Using the established simultaneous quantitative test method, artificial sweeteners were tested in foods such as dairy products, snacks and chocolate. The results calibration curve showed good linearity with high regression coefficients and the result of recovery test showed satisfactory recoveries within 80~110 %.