• Title/Summary/Keyword: Photodiode array(PDA)

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Study on the Marker Steroids of New Zealand Deer (Cervus elaphus var. scoticus) Velvet Antler by UPLC-MS/MS and HPLC-PDA Methods - (II)

  • Lee, Nam Kyung;Jang, Kyoung Hwa;Lee, Jong Tae;Park, Hee Won;Han, Sung Tai;In, Gyo
    • Natural Product Sciences
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    • v.25 no.1
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    • pp.49-58
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    • 2019
  • Eleven steroid hormones (SHs: androstene-3,17-dione, estrone, ${\beta}$-estradiol, ${\alpha}$-estradiol, testosterone, dehydroepiandrosterone, $17{\acute{a}}$-hydroxyprogesterone, medroxyprogesterone, megestrol acetate, progesterone, and androsterone) were detected from New Zealand deer (Cervus elaphus var. scoticus) velvet antler (NZA, 鹿茸 ). A method for the quantification of eleven SHs was established by using ultraperformance liquid chromatography (UPLC)-MS/MS. The linearities ($R^2$ > 0.991), limits of quantification (LOQ values, 0.3 ng/mL to 23.1 ng/mL), intraday and interday precisions (relative standard deviation: RSD < 2.43%), and recovery rates (97.3% to 104.6%) for all eleven SHs were determined. In addition, a method for the quantification of three 7-oxycholesterols (7-O-CSs: 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol) in the NZA was established by using an HPLC-photodiode array (PDA) method. The linearities ($R^2$ > 0.999), LOQ values (30 ng/mL to 350 ng/mL), intraday and interday precisions (RSD < 1.93%), and recovery rates (97.2% to 103.5%) for the three 7-O-CSs were determined. These quantitative methods are accurate, precise, and reproducible. As a result, it is suggested that the five steroid compounds of androstene-3,17-dione, androsterone, 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol could be marker steroids of NZA. These methods can be applied to quantify or standardize the marker steroids present in NZA.

Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation (HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증)

  • Yun, Hyeong-Jun;Yun, So-Mi;Lee, Myoung-Heon;Son, Seong-Wan
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.33-38
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    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).

Contents of Poncirin and Naringin in Fruit of Poncirus Trifoliata according to Different Harvesting Times and Locations for Two Years (2년 동안 지실의 채취시기 및 지역에 따른 Poncirin과 Naringin의 함량)

  • Lee, Sul-Lim;Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.42 no.2
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    • pp.138-143
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    • 2011
  • A high performance liquid chromatography (HPLC) method was developed for simultaneous determination of two major flavonoid glycosides (poncirin and nanringin) in Poncirus trifoliata Raf. by different harvesting times and locations for two years. A SunFire $C_{18}$ column (4.6 mm${\times}$250 mm, 5 ${\mu}M$) was used at $40^{\circ}C$ for the determination of poncirin and naringin. The mobile phase using gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. Flow rate was 1.0 mL/min and injection volume was 10 ${\mu}l$. The chromatogram was monitored by photodiode array (PDA) detection at 280 nm for the identification of two flavonoid glycosides in P. trifoliata. The contents of the two components in P. trifoliata ranged from 0.32~13.02%.

Structure Determination of Heishuixiecaoline A from Valeriana fauriei and Its Content from Different Cultivated Regions by HPLC/PDA Analysis

  • Hyejin Cho;Ki Hyun Kim;Sin Hee Han;Hak-Jae Kim;Ik-Hyun Cho;Sanghyun Lee
    • Natural Product Sciences
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    • v.28 no.4
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    • pp.181-186
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    • 2022
  • A germacrane-type sesquiterpenoid was isolated and purified from a methanol extract of the roots of Valeriana fauriei (RVF) through open column chromatography using silica gel. This compound was verified to be heishuixiecaoline A by spectroscopic analysis. This compound was isolated for the first time from RVF. Quantitative analysis of heishuixiecaoline A from RVF cultivated from three different regions (Eumseong, Jinbu, and Jinan regions) was performed by combining high-performance liquid chromatography with a photodiode array detector. The extract of RVF cultivated in the Jinbu region showed the highest content (9.23 mg/g). In addition, a significant amount of the compound was detected in all RVF samples, which could be expected since it is a characteristic compound of RVF. The sesquiterpenoid group heishuixiecaoline A was isolated from RVF, a resource for various pharmacological substances, and quantitative analysis of RVF cultivated from three different regions was performed. As a result of these experiments, basic data on RVF that can be used in the development and application of pharmaceuticals and health functional foods in the future were obtained.

Simultaneous Analysis of Bangpungtongseong-san and Its Antioxidant Effect (방풍통성산의 동시분석 및 항산화 효능 연구)

  • Seo, Chang-Seob;Kim, Ohn Soon;Shin, Hyeun-Kyoo
    • Herbal Formula Science
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    • v.21 no.2
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    • pp.133-143
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    • 2013
  • Objectives : We carry out the simultaneous quantification for quality control of four components in Bangpungtongseong-san (BPTSS) sample. In addition, we assessed the antioxidant effects of BPTSS sample. Methods : The used column for separation and analysis of four compounds was Luna C18 column and column oven temperature was maintained at $40^{\circ}C$. The mobile phase for simultaneous determination consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. High performance liquid chromatography-photodiode array (HPLC-PDA) method for analysis was performed at a flow rate of 1.0 mL/min with PDA detection at 254 and 280 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of BPTSS were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS) and relative electrophoretic mobility (REM). Results : Calibration curves were acquired with $r^2{\geq}0.9999$. The values of limit of detection (LOD) and quantification (LOQ) were 0.06-0.29 ${\mu}g/mL$ and 0.20-0.98 ${\mu}g/mL$, respectively. The amounts of geniposide, liquiritin, baicalin, and glycyrrhizin in BPTSS were 5.06, 7.33, 27.56, and 7.81 mg/g, respectively. The BPTSS showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction (RC50) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by CuSO4. Conclusions : The established HPLC-PDA method will be helpful to improve quality control of BPTSS. In addition, BPTSS has potentials as therapeutic agent on anti-atherosclerosis.

Analysis of Dyes and Mordants of 16~17th Century Textiles Excavated from Daejeon (16~17세기 출토염직품의 염료와 매염제 분석)

  • Baek, Young-Mee;Kwon, Young-Suk;Goto-Doshida, Sumiko;Saito, Masako
    • Journal of Conservation Science
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    • v.28 no.2
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    • pp.119-129
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    • 2012
  • Excavated textiles provide very important research data on the costume culture of the Joseon dynasty. In particular, dyed textiles are indispensable for textile conservation research and for restoration of remains as well as for general costume culture research. Unfortunately, a prolonged burial environment causes the colors to change and gradually fade after excavation. Therefore, it is very difficult to identify the original color. In this study, natural dyed samples of red, yellow, purple and blue were prepared and analyzed using HPLC-PDA. Dyes of colorants extracted from excavated textile remains were analyzed by HPLC. In addition, mordants were analyzed using (SEM-EDX) in order to estimate the original color. The 16~17th Century's three samples were analyzed, sample 1, and 2 from Eunjin Song's Song Mun-Chang excavated at the Songchon-dong in Daejeon, and sample 3 from Yeosan Song's Song, Hee-Jong excavated at the Mokdal-dong in Daejeon. From the HPLC results, alizarin, purpurin, and indigo were detected on sample 1, alizarin and purpurin on sample 2, ellagic acid and indigo on sample 3. Therefore they were dyed with madder and indigo (sample 1), madder (sample2), pomagranted and indigo (sample 3). Al mordant was identified on three samples.

Determination of Niacin in Infant Formula by Solid-phase Clean-up and HPLC with Photodiode Array Detector (고체상 정제 및 HPLC/PDA에 의한 영유아식 중 나이아신의 분석)

  • Hong, Jee-Eun;Kim, Mi-Ran;Cheon, Sang-Hee;Chai, Jung-Young;Park, Eun-Ryong;Mun, Chun-Sun;Gwak, In-Shin;Kim, Ok-Hee;Lee, Kwang-Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.3
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    • pp.359-363
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    • 2009
  • This study was performed to establish a rapid and simple analytical method for niacin (nicotinic acid and nicotinamide) using HPLC. A pretreatment method for the extraction and clean-up of niacin in infant formula sample and an instrumental condition for HPLC were optimized. Niacin was extracted by 5 mM hexanesulfonate with ultrasonication for 30 min. For the clean-up of the sample, the extract was applied to a HLB cartridge, and then niacin was eluted from the cartridge using 5 mL of 80% methanol after washing with 5 mL of n-hexane. The total recoveries were $83{\sim}104%$ and relative standard deviation were in the range of $1.5{\sim}3.5%$ during the extraction and clean-up process. Niacin was determined by gradient elution with sodium hexanesulfonate/methanol buffer as a mobile phase and a photodiode array detector (260 nm). It showed a high linearity between the content of niacin and the peak area ($r^2$=1.000) in the range of $0.02{\sim}10.0$ mg/L of nicotinic acid and nicotinamide. The detection limit was 0.02 mg/L (0.2 mg/kg in the sample). The method was successfully applied for the determination of niacin in infant formula. Total niacin contents were in the range of $53.5{\sim}140.3$ mg/kg.

Determining Anti-impotence drug-like compounds in Food (식품 중 발기부전치료제 및 유사물질의 분석)

  • Choi, Dongmi;Im, Mooheg;Lee, Kyungjin;Kwon, Kwangil;Jeong, Jiyoon;Park, Gunsang;Hong, Mooki;Lee, Chulwon
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.520-526
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    • 2004
  • To determine 6 anti-impotence drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil and hongdenafil in food, simultaneously, high performance liquid chromatography was applied. In the case of solid sample, it was extracted in organic solvents after homogenizing with mortar and pestle. Whereas liquid sample was just diluted in water and then extracted in organic solvents. Maximum lengths of UV for targets have been identified on photodiode array spectra. As results, vardenafil, hongdenafil, hydroxyhomosildenafil, sildenafil, homosildenafil, and tadalafil were eluted in order using $C_{18}$ column in acetonitrile containing phosphoric acid as the mobile phase. The maximum wavelength (${\lambda}_{max}$) was 216 nm for vardenafil, 233 and 282 nm for hongdenafil, 222 and 293 nm for hydroxyhomosildenafil, sildenafil and homosildenafil, and 284 nm for tadalafil. The overall recoveries were ranged from 95% to 109% and the limit of detection was about 0.04 mg/kg at signal/noise>3. Levels of targets in the selected food samples were 1.7 (hongdenafil) ~ 63 (tadalafil) mg/one dose.

Classification and Comparative Analysis of the Contents of Acorus species and Anemone altaica by UPLC-PDA Analysis (UPLC-PDA를 이용한 창포류의 분류 및 함량 분석)

  • Jo, Ji Eun;Lee, A Yeong;Kim, Hyo Seon;Moon, Byeong Cheol;Ji, Yunui;Chun, Jin Mi;Kim, Ho Kyoung
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.279-284
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    • 2013
  • A quantitative method using ultra performance liquid chromatography with a photodiode array detector (UPLCPDA) was established for the analysis of 2 major plant metabolites: ${\beta}$-asarone and ${\alpha}$-asarone from Acorus gramineus, A. tatarinowii, A. calamus and Anemone altaica, and their contents are compared with other herbs of Acorus species. The method was validated according to the International Conference on harmonization (ICH) guideline for validation of analytical procedures with respect to precision, accuracy, and linearity. The average content of ${\beta}$-asarone in Acorus gramineus was significantly higher than that in others, with the second highest concentration observed in A. tatarinowii, and only a trace amounts found in A. calamus and Anemone altaica. In contrast, the average content of ${\alpha}$-asarone in A. calamus was the highest, followed by that in Acorus gramineus and A. tatarinowii. principle component analysis (PCA) confirmed that ${\beta}$-asarone and ${\alpha}$-asarone content differed among the species. These results suggest that this UPLC-PDA method can be considered as good quality control criteria for Acorus gramineus.

Monitoring of Anti-impotence Drugs and Their Analogues in Food (식품 중의 발기부전치료제 및 유사물질 모니터링)

  • Lee, Hyun-Sook;Lee, Joon-Goo;Kim, Jin-Chul;Oh, Jae-Ho;Jang, Young-Mi;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.43 no.6
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    • pp.675-682
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    • 2011
  • This study was conducted to monitor the concentrations of 24 anti-impotence drugs and their analogues in various foods and dietary supplements, with the aim of ensuring the safety of the foods and supplements. The measurements were done in 226 samples using high performance liquid chromatography/photodiode array detector (HPLC/PDA) and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Five male sexual function enhancing products have been detected as follows: acethylvardenafil (21,476 mg/kg; 15 mg/capsule from one sample), sildenafil (52,778 mg/kg, 29 mg/capsule in one sample; 71,535 mg/kg, 48 mg/capsule in one sample), and tadalafil (9,772-55,545 mg/kg, 6-33 mg/capsule in four samples). A sustainable monitoring of anti-impotence drugs and their analogues in various foods and dietary supplement is recommended.