• Title/Summary/Keyword: HPLC detector

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Simultaneous Quantification of Three Marker Compounds in Samultang by HPLC/DAD (HPLC-DAD를 이용한 사물탕 중 3종 성분의 동시분석법 확립)

  • Won, Jin-Bae;Ma, Jin-Yeul;Lee, Jae-Hoon;Ma, Choong-Je
    • Korean Journal of Pharmacognosy
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    • v.40 no.4
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    • pp.298-302
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    • 2009
  • Samultang is one of traditional medicine composed of Paeonia lactiflora, Angelica gigas, Rehmannia glutinosa and Cnidium officinale. To develop simultaneous determination of paeoniflorin, decursin and 5-HMF in Samultang, a high performance liquid chromatography with diode array detector was used. To separate three marker components, Dionex $C_{18}$ column (5 ${\mu}m$, 120 ${\AA}$, 4.6 mm${\times}$150 mm) was used with a gradient elution system of water and methanol. UV wavelength of detector set at 230 nm and 280 nm. This method was validated by linearity, precision test and recovery test. Calibration curves of three standard components were showed good linear regression ($R^2$>0.9973). LOD and LOQ ranged from 0.08 ${\mu}g$/ml to 0.38 ${\mu}g$/ml and 0.25 ${\mu}g$/ml to 1.16 ${\mu}g$/ml, respectively. The relative standard deviations (RSDs) of data of the inter-day and intra-day experiments were less than 0.54% and 0.89%, respectively. The measured results of recovery test were varied from 93.36 to 107.79 with RSD values 0.01~1.45%. The established method was applied for separation of bio-conversion Samultang sample and compared with control sample.

Determination and survey of tetracyclines residue in honey by high performance liquid chromatography (액체크로마토그래피를 이용한 벌꿀 중 테트라싸이클린계 항생물질의 정량분석 및 잔류조사)

  • Lee Sung-Mo;Park Eun-Jeong;Hong Jee-Young;Kim Jung-Im;Lee Jung-Goo;Hwang Hyun-Soon;Kim Yong-Hee
    • Korean Journal of Veterinary Service
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    • v.28 no.3
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    • pp.203-213
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    • 2005
  • Oxytetracycline, tetracycline, chlortetracycline and doxycycline in honey were separated by solid phase extraction (SPE) and determined with high performance liquid chromatography (HPLC) with UV/Visible detector. Analysis was carried out using following conditions: XTerra $C_8$ column $(3.9\times150mm\;i.d. 5{\mu}m)$, mobile phase composed of 0.01M oxalic acid : methanol : acetonitrile (820 : 80 : 100, v/v/v), isocratic pump at a flow rate of 0.9 ml/min. and $50{\mu}l$ of injection volume, UV/Visible detector with wavelength of 360nm. The calibration curves of four tetracyclines showed linearity $(\gamma^2>0.999)$ at concentration range of $100\~1,000 ng/ml$. The recoveries in fortified honey represented more than $70\%$ with low coefficient of variation $(<10\%)$ for concentration range of four tetracyclines. The detection limits for oxytetracycline, tetracycline, chlortetracycline and doxycycline were 13.8, 14.6, 26.2 and 24.9ng/g in acacia honey. respectively. We also monitored tetracyclines residue in domestic honey [n : 38, acacia (20), wild flower (18) ] and foreign honey [n=22, legally distributed (13), illegally distributed (9)] using modified Charm II screening and HPLC confirmation methods. Seven of the 60 samples $(11.7\%)$ were suspect positive using modified Charm II screening test. Chlortetracycline residue was found in one foreign honey (illegally distributed) tested at concentrations of 0.22 ppm. Conclusively, for more effective control of tetracyclines used in beekeeping should be further survey for residues in honey and also national guidelines (maximum residue limit : MRL) and methods should be obligatory.

Oxidative Cleavage Products of ${\zeta}-Carotene$ (${\zeta}-Carotene$의 산화개열산물)

  • Kim, Seon-Jae
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.985-990
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    • 2000
  • ${\zeta}-Carotene$ was subjected to ozonolysis in ice-cold dichloromethane. The ozonolysis products were fractionated with a silica column and the carbonyl fraction was analyzed by ODS-HPLC with a photodiode array detector. ${\zeta}-Carotene$ was solubilized in toluene, and then oxidized by incubating at $37^{\circ}C$, 72 hr under atmospheric oxygen. Carbonyl compound and acidic compound were produced. In comparison with autoxidation and ozonolysis, each compound showed the same retention time and UV-vis spectra were identical to the reference cleavage products prepared by ozonolysis of ${\zeta}-carotene$. Absorption spectrum of acidic compound was similar to that of standard 4,5-didehydrogeranyl geranyl acid which is known to possess biological activity. Thus, eccentric cleavage of ${\zeta}-carotene$ was confirmed to occur in vitro under oxidation condition.

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Analytical Study for an Acrylic Coating (아크릴 코팅의 성분 분석 연구)

  • Kim, Seog-Jun
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.98-107
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    • 2004
  • In this study, $^1H$ NMR spectroscopy and HPLC were used to identify the type and quantity of each component in an acrylic coating materials applied for an automotive part. By the $^1H$ NMR analysis, it was found that this acrylic coating contained about 88.40 wt% of poly methyl methacrylate (PMMA), 7.05 wt% of methyl methacrylate (MMA), and 2.36 wt% of allyl methacrylate. Polymer additives such as a benzotriazole light stabilizer (Hisorb 328), an oxanilide light stabilizer, butylated hydroxy toluene (BHT), and dimethyl phthalate (DMP) were also identified and measured quantitatively from the $^1H$ NMR spectra. However, only two light stabilizers were identified by reverse phase (RP) HPLC analysis using Bondapak C18 column, methanol mobile phase, and a PDA (Photodiode array) detector. The contents of two light stabilizers in the acrylic coating were measured by a quantitative analysis through UV-Vis spectroscopy and compared with the NMR data. The analytical informations from $^1H$ NMR spetra were better than those from HPLC-PDA plot.

Validation and Determination of Glycyrrhizic Acid as a Marker Substance in Bu-Zhong-Yi-Qi-Tang by HPLC/DAD (HPLC/DAD에 의한 보중익기탕 중의 글리시리진산 정량분석법의 확립)

  • Baek, Ju-Hyun;Kim, Sun-Min;Ahn, Ji-Won;Cho, Chang-Hee;Oh, Mi-Hyune;Cho, Jung-Hee;Lee, Mi-Kyeong;Kim, Hyo-Jin
    • YAKHAK HOEJI
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    • v.52 no.1
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    • pp.7-11
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    • 2008
  • A high performance liquid chromatographic (HPLC) method for the determination of glycyrrhizic acid was developed for the quality control of traditional herbal medicinal preparation Bu-Zhong-Yi-Qi-Tang (BZYQT), which is well-known herbal medicine used as tonic. RP-HPLC analysis was carried out using Capcell pak $C_{18}$ MG column $(5\;{\mu},\;150{\times}4.6\;mm)$ and a mobile phase consisting of acetonitrile and water containing 0.03% phosphoric acid (pH 2.46) at a flow rate of 1.0 ml/min. The optimum wavelength for the detection of the glycyrrhizic acid was found at 250 nm using diode-array UV/VIS detector. The glycyrrhizic acid in BZYQT shows good linearity $(r^2>0.999)$ in the range of $15\;{\mu}g/ml$ to 500 ${\mu}g/ml$. The limit of detection (LOD) was less than 5 ng and R.S.D for intra-day and inter-day reproducibility was less than 7%. The mean recovery of the glycyrrhizic acid was $97.3{\sim}113.0%$. These results suggest that the developed HPLC method is simple and efficient, and could be contributed for the quality control of commercial BZYQT products.

Determination and Survey of Fluoroquinolones Residue in Chicken Muscle by HPLC with Fluorescence Detector (액체크로마토그래피-형광검출기를 이용한 닭고기 중 플루오로퀴놀론계 항균물질 정량분석 및 잔류조사)

  • 박은정;임지흔;이성모
    • Journal of Food Hygiene and Safety
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    • v.19 no.1
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    • pp.12-18
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    • 2004
  • Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

Simultaneous Determination of Carbohydrates and Organic Acids in Various Cultured Dairy Foods by High-Performance Liquid Chromatography: A Preliminary Study (다양한 낙농 발효유제품에서 HPLC를 이용하여 탄수화물과 유기산의 동시 검출에 관한 연구)

  • Kim, Dong-Hyeon;Hwang, Dae-Geun;Chon, Jung-Whan;Kim, Hyunsook;Kim, Hong-Seok;Song, Kwang-Young;Yim, Jin-Hyuk;Kim, Young-Ji;Kang, Il-Byung;Lee, Soo-Kyung;Seo, Kun-Ho
    • Journal of Dairy Science and Biotechnology
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    • v.33 no.4
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    • pp.263-269
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    • 2015
  • Various carbohydrates (lactose, glucose, and fructose), lactic acid, uric acid, and acetoin were separated on a ZORBAX Carbohydrate Analysis column using the Agilent 1200 HPLC ChemStation$^{TM}$, and were identified according to retention times with 325 Dual Wavelength UV-Vis Detector and Refractive Index Detector with 0.013 N $H_2SO_4$ at a flow rate of 0.8 mL/min. In addition, the lactase activity of four commercial probiotic lactic acid bacteria during 6-hour incubation was determined using a high-performance liquid chromatography (HPLC) method. Among the tested samples, Bifidobacterium animalis subsp. lactis showed the greatest lactase activity, followed by Lactobacillus rhamnosus and Lactobacillus casei, with Streptococcus salivarius subsp. thermophilus showing the lowest activity. Therefore, this HPLC technique shows potential for evaluating the fermentation processes of probiotic lactic acid bacteria and could simultaneously confirm the degree of ripening in various fermented dairy foods within only a half hour.

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Determination of Fructooligosaccharides and Raffinose in Infant Formula by High Performance Liquid Chromatography with Evaporative Light Scattering Detector (HPLC-ELSC를 이용한 조제분유 중 fructooligosaccharides 및 raffinose 분석)

  • Shin, Man-Sub;Park, Jae-Woo;Cho, Mi-Ran;Song, Sung-Ok;Kim, Chun-Sun;Choi, Chun-Bae;Lee, Seoung-Won;Lee, Ki-Woong;Chang, Chi-Hoon;Kwak, Byung-Man
    • Korean Journal of Food Science and Technology
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    • v.38 no.6
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    • pp.725-729
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    • 2006
  • A method was developed for the determination of fructooligosaccharides and raffinose contents in infant formula. The samples were extracted and analyzed by liquid chromatography equipped with carbohydrate column and evaporative light scattering detector. The mobile phase used for the gradient mode was water-acetonitrile, at a flow rate of 1.0mL/min. The method showed a mean recovery of 95-99%, the relative standard deviation obtained in the precision study was 0.774-8.982%, the quantification and detection limits were 25-50mg/L.

Development of an Effective Extraction Method for the Quality Control of Eriobotrae Folium : Determination of Triterpenic Acids (비파엽 품질 비교 분석을 위한 Triterpenic Acid의 추출 방법)

  • Lee, Kyoung-In;Park, Moon-Young;Pyo, Byoung-Sik;Kim, Sun-Min
    • Korean Journal of Pharmacognosy
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    • v.41 no.1
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    • pp.62-66
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    • 2010
  • In result of analysis for the content determination of ursolic acid(UA) and oleanolic acid(OA) in extract of Eriobotryae folium using HPLC with UV detector, UA in chloroform extract of Moo-mok variety was showed highest content(2.7843 mg/g). And OA in ethyl acetate extract of Dae-bang variety was showed highest content(0.5898 mg/g). These result suggest that direct extraction using organic solvent(chloroform or ethyl acetate) was useful method for rapid quantitative analysis of UA and OA without preprocessing such as drying or fractionation.

Simultaneous detection of residual fungicide in Bean Sprouts by Solid-phase Extraction (고체상 추출법에 의한 콩나물 중의 잔류농약 동시 검출)

  • Lee, Myunghwoon;Lee, Taejoon;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.509-514
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    • 1993
  • Benomyl, topsin-M and thiram been known as one of the seed disinfectant. For these studies benomyl, topsin-M and thiram simultaneously had been analyzed by high performance liquid chromatographic method using ODS cartridge, benomyl, topsin-M and thiram was chromatographed using an ODS column and eluent 40% Acetonitrile at a flow rate of 1ml/min. The UV Detector responses at 276nm.

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