• Title/Summary/Keyword: Liquid Liquid Extraction

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Advancing the discovery of bioactive compounds, its extraction and identification from the underexplored mollusc, Cipangopaludina lecythis (W. H. Benson, 1836)

  • Ajit Kumar Ngangbam;Bijayalakshmi Devi Nongmaithem;Vu Trong Dai;Laishram Lenin;Lakshmikanta Khundrakpam;Laiphrakpam Pinky;Precious Irom;H. S. Shekhar Sharma
    • Fisheries and Aquatic Sciences
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    • v.27 no.9
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    • pp.539-551
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    • 2024
  • The enormous diversity of molluscs has provided humans with food, colours, medicines and shells, among other resources. Molluscs have long been utilized in traditional medicine in several countries and they are a valuable source of medical supplies for many diverse communities worldwide. The purpose of this study was to identify and assess Cipangopaludina lecythis bioactive compounds in order to determine the nature of the primary ingredient that gives its medicinal properties. C. lecythis flesh and shell extracts using polar and lipophilic solvents were analyzed using liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS). This study provides the first chemical assessment of flesh and shell-opercula of C. lecythis. Chemical analysis of flesh and shell-opercula of C. lecythis clearly showed the presence of major compounds such as chitin, allantoin, linoleic acid, dihydrotachysterol, cyclotrisiloxane hexamethyl and 6-gingerol besides other minor compounds with bioactive properties of medicinal significance. Overall, this research provides good evidence that C. lecythis produce secondary metabolites with a variety of intriguing pharmacological characteristics. They have also long been a part of traditional medicine in many human cultural groups. Its usage by traditional practitioners to treat a range of human diseases is justified by the presence of numerous medicinally significant bioactive chemicals. However, more research on the bioactive compounds found in snails is necessary to standardize the extraction techniques for their detection, quantification and formulations, to validate their in vivo efficacy, and confirm their safety.

A comparative study on enhanced anti-inflammatory activity of Cannabis root extract prepared by combined processing process (복합가공 과정에 의한 대마 뿌리 추출물의 항염증 활성 증진에 관한 비교 연구)

  • Ga-Ram Yu;Hye-Lin Jin;Da-Hoon Kim;Jay Kyun Noah;Hyuck Kim;Dong-Woo Lim
    • The Journal of Korean Medicine
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    • v.45 no.2
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    • pp.41-54
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    • 2024
  • Objectives: Cannabis root is a medicinal plant that has been used in traditional medicine around the world. However, in previous studies using simple extracts, the biological activity was not relatively prominent compared to other herbal medicines. The aim of the present study is to confirm the enhancement of anti-inflammatory activity and bioactive compound of Cannabis root extract prepared by combined processing process. Methods: A series of processes including repeated steam and dry, fermentation, hydrothermal extraction and ethanol extraction was applied to Cannabis root. The antioxidant content of cannabis root extracts obtained through a combined processing process was investigated by analyzing the total phenolic, tannin, and flavonoid contents. Anti-inflammatory effects were tested in LPS-treated RAW264.7 cells. The anti-inflammatory mechanism was examined by western blot. Finally, the component profile of Cannabis root extract was analyzed using High Performance Liquid Chromatography (HPLC) and Thin layer chromatography (TLC). Results: The cannabis root extract prepared by complex processing process had higher antioxidant and anti-inflammatory effects than simple extract. Total phenolic and tannin contents were significantly increased, and DPPH free radical inhibition activity was strengthened by combined processing process. Increased NO production and iNOS expression in LPS-treated RAW264.7 cells were decreased in a concentration-dependent manner upon extract treatment by complex processing process. Additionally, the Stigmasterol content of Cannabis root extract was increased through a complex processing process. Conclusions: Further research is needed on the mechanisms and substances that exhibit the anti-inflammatory effects of Cannabis roots extract prepared by complex processing process.

Improvement of Total Chrolophill Analytical Methods for the Chlorella Products with Extended Products Types (신 제형 클로렐라제품의 총 엽록소 시혐법 개선)

  • Kim, Yoo-Kyung;Lee, Eun-Suk;Han, Jae-Gab;No, Gi-Me;Lim, Dong-Gil;Jung, Ja-Young;Park, Young-Sig
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.70-75
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    • 2011
  • A new and improved analytical method involving alkaline pyridine extraction was proposed to quantity chlorophyll contents in syrup and candy type chlorella products. The performance of analytical method was compared with the conventional Korea food standard method which involves acetone extraction. The application of sonication chlorophyll extraction form alkaline pyridine sample was also explored. The analytical procedure was validated by evaluating accuracy, precision and reproducibility. For liquid samples, the pyridine extraction method showed higher accuracy and precision compared to acetone extraction method. The CV values of pyridine extract method and the acetone extraction method were 18.82 and 40.0, and the accuracy to theoretical values were 106.3% and 78.1%, respectively. When sonication extraction method was applied to the pyridine extraction, the precision was improved as indicated by reduced CV values from 18.82 to 11.36. The improved performance of pyridine-sonication extraction was also validated by recovery test of chlorophyll that was previously spiked into the sample matrix. For solid matrix, the pyridine extraction method showed better performance in analysis of chlorophyll in solid food matrix (CV = 7.05) compared to conventional acetone extraction method (CV = 30.0). However, the accuracy to theoretical values of pyridine and acetone extraction methods only showed only 62.7% an 40%, respectively. The relatively low accuracy of pyridine extraction method (62.7%) was improved to 99.4% by applying additional sonication extraction method. The improved performance of applying additional sonication extraction was validated by standard deviation, CV values and accuracy to theoretical values.

Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

  • Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.85-93
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    • 2016
  • A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

Quantification of seleno proteins in Korean blood serum using solid phase extraction and affinity chromatography-inductively coupled plasma/mass spectrometry (고체상 추출과 친화 크로마토 그라피-유도결합 플라즈마 질량분석법을 이용한 한국인 혈청에서의 셀레노 단백질 정량)

  • Ahn, Ji-Yun;Kwon, Hyo-Sik;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.27 no.2
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    • pp.92-99
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    • 2014
  • Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

Separation and Purification of 2,6-dimethylnaphthalene in the Light Cycle Oil(I) -Concentration of a mixture of dimethylnaphthalene isomers in the light cycle oil- (접촉분해경유에 함유된 2,6-dimethylnaphthalene의 분리, 정제(I) -접촉분해경유에 함유된 dimethylnaphthalene이성체 혼합물의 농축-)

  • Kim, Su-Jin;Kim, Sang-Chai;Kawasaki, Junjiro
    • Applied Chemistry for Engineering
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    • v.7 no.1
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    • pp.162-170
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    • 1996
  • Light cycle Oil(LCO) contains 2,6-dimethylnaphthalene (2,6-DMNA) which is used as the basic material for high performance engineering plastics and liquid crystal polymer. This study was experimentally investigated to concentrate a mixture of dimethylnaphthalene(DMNA) isomers in the LCO by extraction-distillation combination as a pretreatment for separation and purification of 2,6-DMNA in the LCO. Furthermore, concentration of a mixture of DMNA isomers in the LCO compared between distillation and extraction-distillation combination. The recovery of aromatics in the LCO was performed by batch cocurrent multistage extraction with dimethylsulfoxide and water mixture as solvent. The concentration of naphthalene group(carbon number 10-12) in the extracted mixture is higher than that in the LCO. The yield for naphthalene group increased with decreasing carbon number. The yield for a mixture of DMNA isomers obtained in 5 equilibrium extration runs was about 65%. the separation of individual components with extractedmixture was tested by batch distillation. Futhermore, for recovery of a mixture of DMNA isomers of high concentration, distillate containing DMNA was distilled. As a result, a mixture of DMNA isomers with high concentration such as 60wt% was recovered. The extraction-distillation combination was more effective than the distillation to concentration a mixture of DMNA isomer in the LCO.

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Comparison of Major Compounds in Illicii Veri Fructus by Extraction Solvents (추출용매에 따른 팔각회향의 주성분 함량비교)

  • Lee, A Yeong;Kim, Hyo Seon;Choi, Goya;Chun, Jin Mi;Moon, Byeong Cheol;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.28 no.6
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    • pp.47-51
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    • 2013
  • Objectives : The Illicii Veri Fructus was not only traditional medicine but also food in Asia. The aim of this study was selection of optimum solvent in the fruit of Illicii Veri Fructus because an appropriate solvent affect a medicinal effect. Methods : Illicii Veri Fructus was carried out ultrasonic-assisted extraction as various solvents. Two main compounds, p-anisaldehyde and anethole, were successfully analyzed by high performance liquid chromatography-photodiode array detector (HPLC-PDA) and carried out method validation according to ICH guideline. The optimum solvent selected by comparing with yields of two main ingredients. Results : The p-anisaldehyde and anethole were detected at approximately 8.0 min and 19.8 min, respectively. It was all below 5.0% that RSD of retention time and peak area for two main peaks. Calibration curves of two compounds were good linearity as $R^2$ >0.9999. All of the precisions and accuracy were good intra-day and inter-day as below 5.0% RSD. Limited of detection (LOD) of p-anisaldehyde and anethole were analyzed as $0.134{\mu}g/mL$ and $4.286{\mu}g$, respectively. Limited of quantification (LOQ) of two compounds were $0.407{\mu}g$ and $12.989{\mu}g$, respectively. As a result of this study, p-anisladehyde was detected as 0.209 ~ 0.467%, however anethole was not detected in the distilled water. Conclusions : Anethole was main component as 5.329 ~ 6.815% except for water extraction. Methanol extraction among various solvents was detected the highest contents of p-anisaldehyde and anethole as 0.467(${\pm}0.008$)% and 6.815(${\pm}0.220$)%, respectively.

Determination of Domoic Acid in Seafood Matrices using HPLC-UV with Solid Phase Extraction Cleanup (고체상 추출 전처리 및 HPLC-UV를 이용한 수산물 중 domoic acid의 분석)

  • Si Eun Kim;Sang Yoo Lee;Ji Eun Park;Hyunjin Jung;Hyang Sook Chun
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.297-304
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    • 2023
  • Domoic acid (DA), a neurotoxin produced naturally by diatoms, is responsible for incidents of amnesic shellfish poisoning. In this study, a modified analytical method was established to determine domoic acid in seafood using solid phase extraction cleanup and optimizing the amount of sample and extraction solvent to reduce interference effects. The modified method using high-performance liquid chromatography with ultraviolet detection was validated using three seafood matrices (mussel, red snow crab, and anchovy) at three concentrations (1, 2, and 4 mg/kg) and compared to the Food Code method. Compared to the Food Code method, the modified method showed better performance in terms of linearity (R2>0.999), detection limit (0.02-0.03 mg/kg), quantification limit (0.05-0.09 mg/kg), intra-/inter-day accuracy (86.2-100.4%), and intra-/inter-day precision (0.2-4.0%). Furthermore, the method was successfully applied for the analysis of 87 seafood samples marketed in Korea, and DA was detected at a low concentration of 140 ㎍/kg in one anchovy sample. These results suggest that the modified method can be used for routine determination of DA in seafood.

A Study on Optimization for Separation of Phenols and Preconcentration-Separation of Trace Phenols in Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에서 페놀류의 분리 최적화 및 미량 페놀류의 농축-분리에 관한 연구)

  • Lee Dai Woon;Lee Sung Won;So, Min Jeong;Cho Byung Yun
    • Journal of the Korean Chemical Society
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    • v.37 no.5
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    • pp.513-522
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    • 1993
  • The purpose of this study is to optimize the selectivity of mobile phase solvents for separation of 25 phenols in reversed phase liquid chromatography and to accomplish the simultaneous preconcentration and separation of trace phenols from water samples. Phenols used in this study were classified into three groups, chloro-, methyl-, and nitrophenols. Quaternary solvent mobile phases were employed to improve the selectivity. Overlapping resolution maps(ORM) as a statistical simplex techniques was used to predict the optimum solvent system. Additional criterion such as pH and temperature were also investigated. In order to improve the resolution and decrease the analysis time, isoselective multisolvent gradient elution system was employed with ORM-Prism method. The simultaneous preconcentration and separation of trace phenols from water samples were performed by using XAD-2/Dowex 1-X8 tandem column. When the extraction efficiency was evaluated by sampling up to 1 L of distilled water, recovery of the phenols, except phenol, was above 90% and the limit of detection of the phenols was 5 ppb. The XAD-2/Dowex 1-X8 method was superior to C18 cartridge in terms of recovery and selectivity.

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