• Title/Summary/Keyword: Liquid-Liquid Extraction

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Removing Lipemia in Serum/Plasma Samples: A Multicenter Study

  • Castro-Castro, Maria-Jose;Candas-Estebanez, Beatriz;Esteban-Salan, Margarita;Calmarza, Pilar;Arrobas-Velilla, Teresa;Romero-Roman, Carlos;Pocovi-Mieras, Miguel;Aguilar-Doreste, Jose-Angel;Commission on Lipoprotein and Vascular Diseases, Sociedad Espanola de Quimica Clinica
    • Annals of Laboratory Medicine
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    • v.38 no.6
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    • pp.518-523
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    • 2018
  • Background: Lipemia, a significant source of analytical errors in clinical laboratory settings, should be removed prior to measuring biochemical parameters. We investigated whether lipemia in serum/plasma samples can be removed using a method that is easier and more practicable than ultracentrifugation, the current reference method. Methods: Seven hospital laboratories in Spain participated in this study. We first compared the effectiveness of ultracentrifugation ($108,200{\times}g$) and high-speed centrifugation ($10,000{\times}g$ for 15 minutes) in removing lipemia. Second, we compared high-speed centrifugation with two liquid-liquid extraction methods-LipoClear (StatSpin, Norwood, USA), and 1,1,2-trichlorotrifluoroethane (Merck, Darmstadt, Germany). We assessed 14 biochemical parameters: serum/plasma concentrations of sodium ion, potassium ion, chloride ion, glucose, total protein, albumin, creatinine, urea, alkaline phosphatase, gamma-glutamyl transferase, alanine aminotransferase, aspartate-aminotransferase, calcium, and bilirubin. We analyzed whether the differences between lipemia removal methods exceeded the limit for clinically significant interference (LCSI). Results: When ultracentrifugation and high-speed centrifugation were compared, no parameter had a difference that exceeded the LCSI. When high-speed centrifugation was compared with the two liquid-liquid extraction methods, we found differences exceeding the LCSI in protein, calcium, and aspartate aminotransferase in the comparison with 1,1,2-trichlorotrifluoroethane, and in protein, albumin, and calcium in the comparison with LipoClear. Differences in other parameters did not exceed the LCSI. Conclusions: High-speed centrifugation ($10,000{\times}g$ for 15 minutes) can be used instead of ultracentrifugation to remove lipemia in serum/plasma samples. LipoClear and 1,1,2-trichlorotrifluoroethane are unsuitable as they interfere with the measurement of certain parameters.

Preparation of High Purity Ammonium Dinitramide and Its Liquid Mono-propellant (암모늄 디나이트라마이드염의 합성 및 액상연료화 연구)

  • Kim, Wooram;Park, Mijeong;Kim, Sohee;Jeon, Jong-Ki;Jo, Youngmin
    • Applied Chemistry for Engineering
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    • v.30 no.5
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    • pp.591-596
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    • 2019
  • A recently developed propellant, ammonium dinitramide (ADN, $NH_4N(NO_2)_2$ is stable and safe at an ambient condition. However, it requires high purity for practical applications. A very little quantity of foreign impurities in ADN may cause clogging of thruster nozzles and catalyst poisoning for the use of a liquid propellant. Thus, several purification processes for precipitated ADN particles such as repetition extraction, activated carbon adsorption and low-temperature extraction were presented in this study. The purifying methods helped to improve the chemical purity as evaluated by FT-IR and UV-Vis spectroscopy in addition to ion chromatography (IC) analyses. Among the purification processes, adsorption was found to be the best, showing a final purity of 99.8% based on relative quantification by IC. Thermal analysis revealed an exothermic temperature of $148^{\circ}C$ for the synthesized liquid monopropellant, but rose to $188^{\circ}C$ when urea was added.

Liquid chromatography-tandem mass spectrometric analysis of oleracone D and its application to pharmacokinetic study in mice

  • Lim, Dong Yu;Lee, Tae Yeon;Lee, Jaehyeok;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.193-201
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    • 2021
  • We have demonstrated a sensitive analytical method of measuring oleracone D in mouse plasma using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Oleracone D and oleracone F (internal standard) in mouse plasma samples were processed using a liquid-liquid extraction method with methyl tertbutyl ether, resulting in high and reproducible extraction recovery (80.19-82.49 %). No interfering peaks around the peak elution time of oleracone D and oleracone F were observed. The standard calibration curves for oleracone D ranged from 0.5 to 100 ng/mL and were linear with r2 of 0.992. The inter- and intra-day accuracy and precision and the stability fell within the acceptance criteria. The pharmacokinetics of oleracone D following intravenous and oral administration of oleracone D at doses of 5 mg/kg and 30 mg/kg, respectively, were investigated. When oleracone D was intravenously injected, it had first-order elimination kinetics with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 0.95 %, with multi-exponential kinetics. The low aqueous solubility and a high oral dose of oleracone D may explain the different elimination kinetics of oleracone D between intravenous and oral administration. Collectively, this newly developed sensitive LC-MS/MS method of oleracone D could be successfully utilized for investigating the pharmacokinetic properties of this compound and could be used in future studies for the lead optimization and biopharmaceutic investigation of oleracone D.

Liquid Chromatography-Tandem Mass Spectrometric Analysis of Nannozinone A and Its Application to Pharmacokinetic Study in Mice

  • Lee, Chul Haeng;Kim, Soobin;Lee, Jaehyeok;Jeon, Ji-Hyeon;Song, Im-Sook;Han, Young Taek;Choi, Min-Koo
    • Mass Spectrometry Letters
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    • v.12 no.1
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    • pp.21-25
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    • 2021
  • We aimed to develop and validate a sensitive analytical method of nannozinone A, active metabolite of Nannochelins A extracted from the Myxobacterium Nannocytis pusilla, in mouse plasma using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Mouse plasma samples containing nannozinone A and 13C-caffeine (internal standard) were extracted using a liquid-liquid extraction (LLE) method with methyl tert-butyl ether. Standard calibration curves were linear in the concentration range of 1 - 1000 ng/mL (r2 > 0.998) with the inter- and intra-day accuracy and precision results less than 15%. LLE method gave results in the high and reproducible extraction recovery in the range of 78.00-81.08% with limited matrix effect in the range of 70.56-96.49%. The pharmacokinetics of nannozinone A after intravenous injection (5 mg/kg) and oral administration (30 mg/kg) of nannozinone A were investigated using the validated LC-MS/MS analysis of nannozinone A. The absolute oral bioavailability of nannozinone A was 8.82%. Plasma concentration of nannozinone A after the intravenous injection sharply decreased for 4 h but plasma concentration of orally administered nannozinone A showed fast distribution and slow elimination for 24 h. In conclusion, we successfully applied this newly developed sensitive LC-MS/MS analytical method of nannozinone A to the pharmacokinetic evaluation of this compound. This method can be useful for further studies on the pharmacokinetic optimization and evaluating the druggability of nannozinone A including its efficacy and toxicity.

Simultaneous Analysis Method for 27 Endocrine Disrupting Chemicals in Human Urine using UPLC-MS/MS (UPLC-MS/MS를 이용한 소변 시료 중 내분비계 교란물질 27종 동시분석법 확립)

  • Subeen Park;Na-youn Park;Younglim Kho
    • Journal of the Korean Chemical Society
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    • v.68 no.4
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    • pp.191-198
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    • 2024
  • Endocrine disrupting chemicals (EDCs) are compounds that come from outside the body and disrupt hormone action within the body's endocrine system. Examples include parabens, benzophenones, bisphenols, and phthalates, which are currently used in a wide range of applications. However, continuous exposure to them can have negative effects on glycemic control, reproduction, metabolism, nervous system development, pregnancy, childbirth, and growth. In this study, human samples (urine) were pretreated using liquid-liquid-extraction to determine the exposure level of EDCs and then analyzed effectively and rapidly by UPLC-MS/MS. In this way, the analytical conditions were established and the reliability of the simultaneous analysis method was evaluated through method validation. The results showed that the accuracy ranged from 75.28 to 122.36% and the precision ranged from 2.16 to 22.74%. The analytical method established in this study can be used as a methodology for future studies to evaluate and monitor the exposure of EDCs in human samples.

The Comparative Study on Compositional Pattern Analysis of Decoction of Extracted Artemisia argyi by Different Extraction Time (전탕 시간에 따른 애엽의 성분패턴 비교연구)

  • Yoon, Jun-Geol;Kim, Mean-Sun;Han, Seong-Min;Hwang, Deok-Sang;Lee, Jin-Moo;Lee, Chang-Hoon;Jang, Jun-Bock
    • The Journal of Korean Obstetrics and Gynecology
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    • v.33 no.2
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    • pp.1-12
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    • 2020
  • Objectives: This study was conducted to find out the optimal extraction time for Artemisia argyi. Methods: The compositional pattern was compared with HPLC (High Performance Liquid Chromatography) and GC (Gas-Chromatography) by decocting Artemisia argyi 10, 60, 120 minutes respectively. Results: With longer extraction time, the contents of reference compounds were extracted 1.1 times more when 3,4-dicaffeoylquinic acid was extracted for 60 minutes than when extracted for 10 minutes in HPLC test, but the contents were reduced when extracted for 120 minutes compared to 60 minutes extraction time. 3,4-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, 4,5-di-O-caffeoylquinic acid, jaceosidin, and eupatilin showed the largest yield rate when extracted for 10 minutes, and it decreased as time passed. The contents of chlorogenic acid, 3,5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, jaceosidin, scoparone, and eupatilin were detected only in 10 minutes extraction but not in 60 or 120 minutes extraction according to GC test. Conclusions: The results show that extraction time could affect the physicochemical characteristic or composition of Artemisia argy extracted. Thus, short extraction time could be useful for decoction of Artemisia argyi.

Ash Reduction and the Change of Fuel Properties for Spent Mushroom Substrates by Acid Solution Extraction (산(acid) 첨가 용매 추출에 의한 폐버섯배지 회분 감소 및 연료특성 변화)

  • Lee, Eun-Jee;Oh, Doh-gun;Kim, Sun-Mee;Park, Eun-Suk;We, Sung-Gook
    • Korean Chemical Engineering Research
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    • v.48 no.3
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    • pp.365-374
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    • 2010
  • The ash reduction effects and fuel property changes of spent mushroom substrates by acid solution extraction, and the production possibilities of wood pellet fuel using them were studied. The ash weight of spent Pleurotus eryngii substrates was reduced from 8.81%(w/w) to 3.33%(w/w), and calorific value was increased from 3,958.3 kcal/kg to 4219.2 kcal/kg when extracted with a mixture of Acetic acid 2%(w/w) and Anhydrous citric acid 1%(w/w) in condition of liquid ratio 1:8, extraction temperature $55^{\circ}C$ and extraction time 180 min. The ash weight of spent Flammulina velutipes substrates was reduced from 14.91%(w/w) to 4.07%(w/w), and calorific value was increased from 4,190.3 kcal/kg to 4,219.2 kcal/kg when extracted with a mixture of Acetic acid 3%(w/w) and Anhydrous citric acid 1%(w/w) in condition of liquid ratio 1:8, extraction temperature $65^{\circ}C$ and extraction time 180 min. The ash weight of spent Pleurotus osteratus substrates was reduced from 3.31%(w/w) to 0.59%(w/w), and the smallest reduction was in calorific value from 4,558.6 kcal/kg to 4,216.2 kcal/kg when extracted with a mixture of Acetic acid 1%(w/w) and Anhydrous citric acid 1%(w/w) in condition of liquid ratio 1:8, extraction temperature $65^{\circ}C$ and extraction time 180 min.