• 제목/요약/키워드: Salting-out extraction technique

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Salting-out extraction of ginsenosides from the enzymatic hydrolysates of Panax quinquefolium based on ethanol/sodium carbonate system

  • Wei, Yingqin;Hou, Baojuan;Fang, Haiyan;Sun, Xinjie;Ma, Feng
    • Journal of Ginseng Research
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    • 제44권1호
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    • pp.44-49
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    • 2020
  • Background: Salting-out extraction (SOE) had been developed as a special branch of aqueous two-phase system recently. So far as we know, few reports involved in extracting ginsenosides with SOE because of the lower recovery caused by the unique solubility and surface activity of ginsenosides. A new SOE method for rapid pretreatment of ginsenosides from the enzymatic hydrolysates of Panax quinquefolium was established in this article. Methods: The SOE system comprising ethanol and sodium carbonate was selected to extract ginsenosides from the enzymatic hydrolysates of Panax quinquefolium, and HPLC was applied to analyze the ginsenosides. Results: The optimized extraction conditions were as follows: the aqueous two-phase extraction system comprising ethanol, sodium carbonate, ethanol concentration of 41.51%, and the mass percent of sodium carbonate of 7.9% in the extraction system under the experimental condition. Extraction time had minor influence on extraction efficiency of ginsenosides. The results also showed that the extraction efficiencies of three ginsenosides were all more than 90.0% only in a single step. Conclusion: The proposed method had been successfully applied to determine ginsenosides in enzymatic hydrolysate and demonstrated as a powerful technique for separating and purifying ginsenosides in complex samples.

5원자 헤테로고리 화합물을 이용한 $Mg^{2+}$의 정량 (Determination of $Mg^{2+}$ using 5-membered Heterocyclic Compound)

  • 서무룡;이심성;김재상;박태명
    • 분석과학
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    • 제6권3호
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    • pp.307-311
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    • 1993
  • 5원자 헤테로고리를 포함하는 열린고리형의 ionophore를 합성하였다. 이 때 합성한 ionophore를 착화제로 이용하여 수용액 중의 $Mg^{2+}$을 염석추출법으로 추출하여 원자 흡광 광도법으로 정량하였다. Acetate 완충용액으로 pH를 4.2로 조절한 $Mg^{2+}$를 포함하는 수용액에 ionophore-AN 용액을 넣어 $Mg^{2+}$-ionophore 착물을 형성시킨 다음, 염석제를 첨가하여 유기층으로 추출하고, 유기층의 착물의 흡광도를 원자 흡광 광도계로서 측정하여 $Mg^{2+}$를 정량하였다. 최적 추출 조건을 조사해 본 결과, 최적 pH는 2.5~5.0이었으며, 염석제인 황산암모늄[$(NH_4)_2SO_4$]의 양은 5g 이상이면 정량적으로 추출되었다. 또한 $Mg^{2+}$과 ionophore의 착물 조성비는 1:2이었다. $Mg^{2+}$의 정량범위는 0.24ppm~2.4ppm이었으며 $Ca^{2+}$이온 및 EDTA의 방해효과가 크게 나타났다.

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Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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    • pp.3444-3450
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    • 2013
  • Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

아세토니트릴 용매 중에서 Copper-1,5,9,13-Tetrathiacyclohexadecane착물의 전기화학적 거동과 그 분석적 응용 (Electrochemical Behaviors and Analytical Application of Copper-1,5,9,13-Tetrathiacyclohexadecane Complex in Acetonitrile)

  • 서무룡;이부영;최명자;배준웅;박태명
    • 대한화학회지
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    • 제36권3호
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    • pp.412-418
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    • 1992
  • 비수용매인 아세토니트릴 중에서 Cu(Ⅱ)와 1,5,9,13-tetrathiacyclohexadecane[16-ane-$S_4$]의 착물에 대한 전기화학적 거동으로서 직류폴라로그램과 미분펄스폴라로그램으로부터 환원전류의 유형과 가역성을 조사하고, 이들 화합물의 분석적 응용으로서 수용액에 있는 Cu(Ⅱ) 이온을 염석추출법으로 정량하였다. 또한 아세토니트릴 용매 중에서 착물의 안정도 상수를 구하고, 분석적 응용으로 수용액 중의 Cu(Ⅱ)를 염석추출법으로 정량하기 위하여 추출조건, 곧 킬레이트와 염석제의 효과, pH 범위를 구하고 또한 Cu(Ⅱ) 이온을 정량하는데 있어서의 검량성과 공존이온 효과를 조사하였다. 실험결과로부터 환원 과정은 비가역적이었으며 환원전류는 확산지배적임을 알았다. 또한 아세토닐트릴 용매 중에서 착물의 log $K_f$의 값은 3.51이었으며 Cu(Ⅱ) 이온을 정량하는데 있어 공존하는 이온의 영향을 별로 받지 않아 선택성이 좋았으며 본 실험방법에 의한 정량한계는 60ppb 이었다.

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Receptor activator of nuclear factor kappa-B gene polymorphisms in Iranian periodontitis and peri-implantitis patients

  • Kadkhodazadeh, Mahdi;Baghani, Zahra;Ebadian, Ahmad Reza;Kaghazchi, Zahra;Amid, Reza
    • Journal of Periodontal and Implant Science
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    • 제44권3호
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    • pp.141-146
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    • 2014
  • Purpose: Peri-implantitis and periodontitis are inflammatory and infectious diseases of implant and tooth-supporting tissues. Recently, the role of gene polymorphisms of immune response components in the relevant pathogenesis has been investigated. The present study was the first to evaluate the relationship between two known single nucleotide polymorphisms (SNPs) of the receptor activator of nuclear factor kappa-${\beta}$ (RANK) gene (rs3018362 and rs35211496) in chronic periodontitis and peri-implantitis patients in an Iranian population. Methods: Eighty-one periodontally healthy patients, 38 patients with peri-implantitis, and 74 patients with chronic periodontitis were enrolled in this study. DNA was extracted from blood arm vein samples by using Miller's salting out technique according to the manufacturer's instructions given in the extraction kit. The concentration of DNA samples was measured using a spectrophotometer. The genetic polymorphisms of the RANK gene were evaluated using a competitive allele specific polymerase chain reaction (KBioscience allele specific PCR) technique. Differences in the frequencies of genotypes and alleles in the diseased and healthy groups were analyzed using chi-squared statistical tests (P<0.05). Results: Analysis of rs35211496 revealed statistically significant differences in the expression of the TT, TC, and CC genotypes among the three groups (P=0.00). No statistically significant difference was detected in this respect between the control group and the chronic periodontitis group. The expression of the GG, GA, and AA genotypes and allele frequencies (rs3018362) showed no statistically significant difference among the three groups (P=0.21). Conclusions: The results of this study indicate that the CC genotype of the rs35211496 RANK gene polymorphism was significantly associated with peri-implantitis and may be considered a genetic determinant for peri-implantitis, but this needs to be confirmed by further studies in other populations.