• Title/Summary/Keyword: rapid extraction method

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Volatile Aroma Compounds and Their Characteristics of Labiatae by Solid-Phase Microextraction (SPME) (Solid-Phase Microextraction (SPME)에 의한 꿀풀과 약초의 향기성분과 그 특성)

  • Song, Yong-Eun;Ku, Chang-Sub;Mun, Sung-Phil;Ryu, Ji-Sung;Kim, Dae-Hyang;Choi, Joung-Sik;Choi, Yeong-Geun
    • Korean Journal of Medicinal Crop Science
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    • v.10 no.2
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    • pp.120-125
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    • 2002
  • This study was carried out to find the possibility of use of Solid Phase Microextraction (SPME) for extracting the volatile aroma compounds in the five aromatic plants (Agastache rugosa O. Kuntze, Mentha arvensis Linne, Thymus quinquecostatus Celakovsky, Elsholtzia splendens Nakai, Schizonepta tenuifolia Briquet) belongs to the Labiatae. In the result of the analysis, the volatile aroma compounds were mainly composed monoterpene alcohol (linanol, menthol, ${\alpha}-terpineol$, borneol), monoterpene ketone (limonene, menthone) and sesquiterpene (trans-caryophyllene,${\delta}-cadinene)$. The volatile aroma compounds of Agastache rugosa O. Kuntze and Mentha arvensis Linne were extracted by SPME more identified than the SDE. However, Schizonepta tenuifolia Briquet more identified by the SDE and in Elsholtzia splendens Nakai similar to the SDE. Especially, the SPME showed the sesquiterpene contents was more than the SDE. The major volatile aroma compounds were difference but the composition of those between the SPME and the SDE showed no difference. Within the results, the SPME showed the most convenient and a rapid extraction method to analysis of the volatile aroma compounds.

Validated HPLC Method for the Pharmacokinetic Study of Atenolol and Chlorthalidone Combination Therapy in Korean Subjects

  • Kang, Hyun-Ah;Kim, Hwan-Ho;Kim, Se-Mi;Yoon, Hwa;Cho, Hea-Young;Oh, Seaung-Youl;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.5
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    • pp.331-338
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    • 2006
  • A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

Improvement of Determination Method for Propionic Acid in Bakery Products (빵의 프로피온산 함량 분석방법 개선)

  • Lee, Sung-Deuk;Kim, Yeon-Sun;Doo, Ok-Joo;Kim, Mi-Sun;Park, Young-Hae;Kim, Il-Young;Chae, Young-Zoo
    • Journal of Food Hygiene and Safety
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    • v.24 no.4
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    • pp.332-337
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    • 2009
  • Most propionic acid is added to food (especially breads) as preservatives and its form is sodium or calcium salt. Most countries admitted propionic acid as food preservatives but a tolerance limit is somewhat different according to countries. Recoveries of the official method for propionates reported as 50.0~60.0%. Accordingly new rapid determination method for propionates was developed using formic acid added sodium chloride (5 g) and ether (formic acid : ether = 1 : 2) as the extraction solvent to improve the official method with the complex processes. Propionate was dissolved from the samples with formic acid omitting steam distillation and ion exchange procedure. Then propionate in formic acid was extracted with ether and sodium chloride again. A $1\;{\mu}l$ aliquot of the filtrate of ether was analyzed by gas chromatograph. Recoveries from sample A and B fortified with propionic acid sodium salt were 85.0 % and 90.0 %, respectively.

Development of LC-MS/MS analytical methods for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai (LC-MS/MS를 이용한 생약 백출 및 우슬 중 Metalaxyl 잔류분석법 개발)

  • Yun, Myung-Sub;Yang, Seung-Hyun;Choi, Hoon
    • Journal of Applied Biological Chemistry
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    • v.65 no.1
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    • pp.17-21
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    • 2022
  • A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH2) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r2) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

Quantitative PCR for Etiologic Diagnosis of Methicillin-Resistant Staphylococcus aureus Pneumonia in Intensive Care Unit

  • Kwon, Sun-Jung;Jeon, Tae-Hyeon;Seo, Dong-Wook;Na, Moon-Joon;Choi, Eu-Gene;Son, Ji-Woong;Yoo, Eun-Hyung;Park, Chang-Gyo;Lee, Hoi-Young;Kim, Ju-Ock;Kim, Sun-Young;Kang, Jae-Ku
    • Tuberculosis and Respiratory Diseases
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    • v.72 no.3
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    • pp.293-301
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    • 2012
  • Background: Ventilator-associated pneumonia (VAP) requires prompt and appropriate treatment. Since methicillin-resistant Staphylococcus aureus (MRSA) is a frequent pathogen in VAP, rapid identification of it, is pivotal. Our aim was to evaluate the utility of quantitative polymerase chain reaction (qPCR) as a useful method for etiologic diagnoses of MRSA pneumonia. Methods: We performed qPCR for mecA, S. aureus-specific femA-SA, and S. epidermidis-specific femA-SE genes from bronchoalveolar lavage or bronchial washing samples obtained from clinically-suspected VAP. Molecular identification of MRSA was based on the presence of the mecA and femA-SA gene, with the absence of the femA-SE gene. To compensate for the experimental and clinical conditions, we spiked an internal control in the course of DNA extraction. We estimated number of colony-forming units per mL (CFU/mL) of MRSA samples through a standard curve of a serially-diluted reference MRSA strain. We compared the threshold cycle (Ct) value with the microbiologic results of MRSA. Results: We obtained the mecA gene standard curve, which showed the detection limit of the mecA gene to be 100 fg, which corresponds to a copy number of 30. We chose cut-off Ct values of 27.94 (equivalent to $1{\times}10^4$ CFU/mL) and 21.78 (equivalent to $1{\times}10^5$ CFU/mL). The sensitivity and specificity of our assay were 88.9% and 88.9% respectively, when compared with quantitative cultures. Conclusion: Our results were valuable for diagnosing and identifying pathogens involved in VAP. We believe our modified qPCR is an appropriate tool for the rapid diagnosis of clinical pathogens regarding patients in the intensive care unit.

Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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THE USE OF NEAR INFRARED REFLECTANCE SPECTROSCOPY(NIRS) TO PREDICT CHEMICAL COMPOSITION ON MAIZE SILAGE

  • D.Cozzolino;Fassio, A.;Mieres, J.;Y.Acosta
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1610-1610
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    • 2001
  • Microbiological examination of silage is of little value in gauging the outcome of silage, and so chemical analysis is more reliable and meaningful indicator of quality. On the other hand chemical assessments of the principal fermentation products provide an unequivocal basis on which to judge quality. Livestock require energy, protein, minerals and vitamins from their food. While fresh forages provide these essential items, conserved forages on the other hand may be deficient in one or more of them. The aim of the conservation process is to preserve as many of the original nutrients as possible, particularly energy and protein components (Woolford, 1984). Silage fermentation is important to preservation of forage with respect of feeding value and animal performance. Chemical and bacteriological changes in the silo during the fermentation process can affect adversely nutrient yield and quality (Moe and Carr, 1984). Many of the important chemical components of silage must be assayed in fresh or by extraction of the fresh material, since drying either by heat or lyophilisation, volatilises components such as acids or nitrogenous components, or effects conversion to other compounds (Abrams et al., 1987). Maize silage dorms the basis of winter rations for the vast majority of dairy and beef cattle production in Uruguay. Since nutrient intake, particularly energy, from forages is influenced by both voluntary dry matter intake and digestibility; there is a need for a rapid technique for predicting these parameters in farm advisory systems. Near Infrared Reflectance Spectroscopy (NIRS) is increasingly used as a rapid, accurate method of evaluating chemical constituents in cereals and dried forages. For many years NIRS was applied to assess chemical composition in dry materials (Norris et al., 1976, Flinn et al., 1992; Murray, 1993, De Boever et al., 1996, De la Roza et al., 1998). The objectives of this study were (1) to determine the potential of NIRS to assess the chemical composition of dried maize samples and (2) to attempt calibrations on undried samples either for farm advisory systems or for animal nutrition research purposes in Uruguay. NIRS were used to assess the chemical composition of whole - plant maize silage samples (Zea mays, L). A representative population of samples (n = 350) covering a wide distribution in chemical characteristics were used. Samples were scanned at 2 nm intervals over the wavelength range 400-2500 nm in a NIRS 6500 (NIRSystems, Silver Spring, MD, USA) in reflectance mode. Cross validation was used to avoid overfitting of the equations. The optimum calibrations were selected on the basis of minimizing the standard error of cross validation (SECV). The calibration statistics were R$^2$ 0. 86 (SECV: 11.4), 0.90 (SECV: 5.7), 0.90 (SECV: 16.9) for dry matter (DM), crude protein (CP), acid detergent fiber (ADF) in g kg$\^$-1/ on dry matter, respectively for maize silage samples. This work demonstrates the potential of NIRS to analyse whole - maize silage in a wide range of chemical characteristics for both advisory farm and nutritive evaluation.

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Development of a Simultaneous Analysis Method for DDT (DDD & DDE) in Ginseng (인삼 중 DDT(DDD 및 DDE) 분석법의 개발)

  • Kim, Sung-Dan;Cho, Tae-Hee;Han, Eun-Jung;Park, Seoung-Gyu;Han, Chang-Ho;Jo, Han-Bin;Choi, Byung-Hyun
    • Korean Journal of Food Science and Technology
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    • v.40 no.2
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    • pp.123-128
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    • 2008
  • The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

HPLC Analysis and Pharmacokinetics of KAL-1120, a Novel Anti-inflammation Agent, in Rats (흰쥐에서 항염증제 후보물질 KAL-1120의 HPLC 분석 및 약물동태)

  • Shin, Dae-Hwan;Lee, Jung-Yeol;Park, Seong-Hyeok;Lee, Gyeong-Bok;Han, Kun;Chung, Youn-Bok
    • Journal of Pharmaceutical Investigation
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    • v.40 no.2
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    • pp.101-107
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    • 2010
  • A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of N-(-4-Chlorophenyl)-6-hydroxy-7-methoxy-2-chromanecarboxamide (KAL-1120), a novel anti-inflammation agent, in the rat plasma. The method was applied to analyze the compound in the biological fluids such as bile, urine and tissue homogenates. After liquid-liquid extraction, the compound was analyzed on an HPLC system with ultraviolet detection at 275 nm. HPLC was carried out using reversed-phase isocratic elution with a $C_{18}$ column, a mobile phase of a mixture of acetonitril (40 v/v%) at a flow rate of 1.0 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma was linear over the concentration range of 0.05-50 ${\mu}g$/mL. The intra- and inter-day assay accuracies of this method ranged from 0.06% to 9.33% of normal values and the precision did not exceed 6.28% of relative standard deviation. The plasma concentration of KAL-1120 decreased to below the quantifiable limit at 1.5 hr after the i.v. bolus administration of 2-10 mg/kg to rats ($t_{1/2,({\alpha})}$ and $t_{1/2,({\beta})$ of 2.15 and 26.7 min at a dose of 2 mg/kg, 3.91 and 33.0 min at a dose of 10 mg/kg, respectively). The steady-state volume of distribution ($V_{dss}$) and the total body clearance ($CL_t$) were not significantly altered in rats given doses from 2 to 10 mg/kg. Of the various tissues tested, KAL-1120 was mainly distributed in the lung and heart after i.v. bolus administration. KAL-1120 was detected in the bile by 30 min after its i.v. bolus administration. However, the concentration in the urine after i.v. bolus administration became too low to measure, suggesting that KAL-1120 is mostly excreted in the bile. In conclusion, this analytical method was suitable for the preclinical pharmacokinetic studies of KAL-1120 in rats.

Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD (HPLC-UVD를 이용한 농산물 중 pyrifluquinazon 잔류시험법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Kim, Mi-Ra;Lee, Eun-Mi;Kuk, Ju-Hee;Cho, Yoon-Jae;Chang, Moon-Ik;Kwon, Kisung;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.174-181
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    • 2013
  • Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.