• Title/Summary/Keyword: chromatography test

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Simultaneous detection of five biocides in household products by gas chromatography-mass spectrometry

  • Choi, Kyeong-Yun;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.197-204
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    • 2022
  • A gas chromatography-mass spectrometric method was developed for determining 5-chloro-2-methyl-4-isothiazolin-3-one (CMIT), 2-methyl-4-isothiazolin-3-one (MIT), 1,2-benzisothiazolin-3-one (BIT), 3-iodo-2-propynyl butyl carbamic acid (IPBC) and benzoic acid (BA) in household products. A 0.5 g sample was placed in a test tube and dissolved with 5 mL water, 5 mL methylene chloride and 1.0 mL methanol. The solution was extracted by ultra-sonication followed by mechanical shaking using the salting out effect. Under the established condition, the lowest quantification limits of all analytes were in the range of 0.04-10 mg/kg and their relative standard deviations were less than 8.0 %. The method was used to analyze 10 household products. As a result of analyzing 10 household products, MIT was detected in the range of 1.2-3.5 mg/kg in 3 of 10 samples, CMIT was detected in the range of 2.6-8.2 mg/kg in 3 of 10 samples, and BA was detected in the range of 5.0-15 mg/kg in 4 of 10 samples. Meanwhile, BIT and IPBC were not detected in any of the products. It has been shown that this method can be used for the simultaneous determination of biocides with various physical and chemical properties in household products.

Volatile Compounds for Discrimination between Beef, Pork, and Their Admixture Using Solid-Phase-Microextraction-Gas Chromatography-Mass Spectrometry (SPME-GC-MS) and Chemometrics Analysis

  • Zubayed Ahamed;Jin-Kyu Seo;Jeong-Uk Eom;Han-Sul Yang
    • Food Science of Animal Resources
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    • v.44 no.4
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    • pp.934-950
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    • 2024
  • This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

Simultaneous Determination of Four Bioactive Constituents in Galgeun Tang by HPLC/DAD. (HPLC-DAD를 이용한 갈근탕 중 4종 성분의 동시분석법 확립)

  • Won, Jin-Bae;Jeon, Won-Kyung;Ma, Jin-Yeul;Ma, Choong-Je
    • Korean Journal of Pharmacognosy
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    • v.40 no.3
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    • pp.224-228
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    • 2009
  • For the quality control of traditional herbal medicine, Galgeun tang, simultaneous determination of glycyrrhizin, paeoniflorin, puerarin, 6-gingerol was established by using a high performance liquid chromatographic (HPLC) method with diode array detector. To separate five four constituents, DIONEX $C_{18}$ column ($5{\mu}m$, $120{\AA}$, $4.6\;mm{\times}150\;mm$) was used with gradient elution system of water and methanol. Validation of the chromatography method was evaluated by linearity, recovery, and precision test. Calibration curve of standard components showed excellent linearity ($R^2$>0.9906). Limits of detection (LOD) and limits of quantification (LOQ) varied from 0.15 to $0.52{\mu}g$/ml and 0.27 to $0.80{\mu}mg$/ml, respectively. The relative standard deviations (RSDs) of data of the intra-day and inter-day experiments were less than 2.88% and 1.21%, respectively. The results of recovery test were ranged from 96.71 to 106.29% with RSD values 0.01-0.80%.

Multiplication and Antibody Formation of Japanese Encephalitis Virus in Snakes - 1. Antibody responses to the virus and serum

  • Lee, Ho-Wang;Kee, Ryong-Sook
    • The Journal of the Korean Society for Microbiology
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    • v.3 no.1
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    • pp.43-49
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    • 1968
  • Japanese encephalitis(JE) shows its explosive epidemicity in the temperate zone of Asia but little is known on the overwintering mechanism. One of the hypotheses on the overwintering mechanism is that the virus overwinters in the hibernating animals. There has been no report on the proliferation of JE virus(JEV) or antibody formation in the snakes. The purpose of this experiment is to explore the mutual relationship between JEV and snake and to clarify whether JEV proliferates and induce antibody formation in snakes. Three species of non-poisonous common snakes were employed. Precipitation test was carried out after injecting calf serum and, HI and neutralization tests were done by injecting JEV into the snakes. The gamma globulin fraction of pre- and post-injection serum were compared by paper chromatography. According to the results, precipitating antibody reaction to calf serum could be observed only at $4^{\circ}C$. It was failed to demonstrate HI antibody formation but neutralizing antibody could be detected in one of the 9 snakes. Although antibody could not be detected in test-tube, tile result of paper chromatography shows the remarkable increase of gamma globulin fraction after the injection. Above results are strongly indicating the antibody formation in the snakes.

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Purification of hemolysin in mosquitocidal delta-endotoxin from Bacillus thuringiensis subsp. darmstadiensis 73E10-2 (모기유충에 살충력이 있는 Bacillus thuringiensis subsp. darmstadiensis 73E10-2의 내독소의 용혈성 인자의 정제)

  • 김광현;이기희;홍용기
    • Microbiology and Biotechnology Letters
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    • v.19 no.3
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    • pp.303-307
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    • 1991
  • The hemolyic polypeptide in delta-endotoxin from Bacillus thun'ngiensis subsp. darmstadiensis 73ElO-2 was purified by Sephadex G-IOO gel filtration and DEAE-cellulose ion exchange column chromatography. The purity of hemolysin was confirmed by ouchterlony test and SDS-PAGE. The molecular weight of the purified hemolysin was approximately 64 KDa by SDS-PAGE. The purified hemolysin has not mosquitocidal activity against larvae of Aedes agypti, but hemolytic activity on red blood cells of rat. There is no serological relationship between delta-endotoxin from B. thuringiensis subsp. israelensis and the purified hemolysin from the . strain 73ElO-2.

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THE LEVEL OF RESIDUAL MONOMER IN INJECTION MOLDED DENTURE BASE MATERIALS

  • Lee Hyeok-Jae;Kim Chang-Whe;Kim Yung-Soo
    • The Journal of Korean Academy of Prosthodontics
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    • v.41 no.3
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    • pp.360-368
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    • 2003
  • Statement of Problem: The residual monomer of denture base materials causes hypersensitivity on oral mucosa and intereferes with the mechanical properties of the cured resin. The amount of residual monomer is influenced by materials, curing cycle, processing method, and etc. Purpose: The aim of this study was to investigate the residual methyl methacrylate(MMA) content of injection molded denture base polymer, and to compare this with the self-cured resin and the conventional compression molded heat-cured resin. Materials and Methods: Disc shaped test specimens (50mm in diameter and 3mm thick) were prepared in a conventional flasking technique with gypsum molding. One autopolymerized denture base resins (Vertex Sc. Dentimex. Netherlands) and two heat-cured denture base resins (Vertex RS. Dentimex. Netherlands, Ivocap. Ivoclar Vivadent, USA) were used. The three types of specimens were processed according to the manufacturer's instruction. After polymerization, all specimens were stored in the dark at room temperature for 7 days. There were 10 specimens in each of the test groups. 3-mm twist drills were used to obtain the resin samples and 650mg of the drilled sample were collected for each estimation. Gas chromatography (Agillent 6890 Plus Gas Chromatograph, Agillent Co, USA) was used to determine the residual MMA content of 10 test specimens of each three types of polymer. Results: The residual monomer content of injection molded denture base resins was $1.057{\pm}0.141%$. The residual monomer content of injection molded denture base resins was higher than that of compression molded heat cured resin ($0.867{\pm}0.169%$). However, there was no statistical significant difference between two groups (p>0.01). The level of residual monomer in self cured resin($3.675{\pm}0.791$) was higher than those of injection molded and compression molded heat cured resins (p<0.01). Conclusion: With respect to ISO specification pass / fail test (2.2% mass fraction) of residual monomer, injection molding technique($1.057{\pm}0.141%$) is a clinically useful and safe technique in terms of residual monomer.

Anti-nociceptive and anti-inflammatory activities of the essential oil isolated from Cupressus arizonica Greene fruits

  • Fakhri, Sajad;Jafarian, Safoora;Majnooni, Mohammad Bagher;Farzaei, Mohammad Hosein;Mohammadi-Noori, Ehsan;Khan, Haroon
    • The Korean Journal of Pain
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    • v.35 no.1
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    • pp.33-42
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    • 2022
  • Background: Cupressus arizonica Greene is a coniferous tree with great importance in fragrance and pharmaceutical industries. Essential oils from C. arizonica (EC) have shown potential antioxidant, and anti-microbial activities. This study aimed at investigating the anti-nociceptive and anti-inflammatory effects/mechanisms of EC. Methods: The EC was evaluated for anti-nociceptive and anti-inflammatory activities on male Wistar rats using a formalin test and carrageenan-induced paw edema, respectively. Also, we pre-treated some of the animals with naloxone and flumazenil in the formalin test to find out the possible contributions of opioid and benzodiazepine receptors to EC anti-nociceptive effects. Finally, gas chromatography/mass spectrometry (GC/MS) analysis was used to identify the EC's constituents. Results: EC in intraperitoneal doses of 0.5 and 1 g/kg significantly decrease the nociceptive responses in both early and late phases of the formalin test. From a mechanistic point of view, flumazenil administration 20 minutes before the most effective dose of EC (1 g/kg) showed a meaningful reduction in the associated anti-nociceptive responses during the early and late phases of the formalin test. Naloxone also reduced the anti-nociceptive role of EC in the late phase. Furthermore, EC at the doses of 1, 0.5, and 0.25 g/kg significantly reduced paw edema from 0.5 hours after carrageenan injection to 4 hours. GC/MS analysis showed that isolated EC is a monoterpene-rich oil with the major presence of α-pinene (71.92%), myrcene (6.37%), δ-3-carene (4.68%), β-pinene (3.71%), and limonene (3.34%). Conclusions: EC showed potent anti-nociceptive and anti-inflammatory activities with the relative involvement of opioid and benzodiazepine receptors.

Evaluation of the antinociceptive activities of natural propolis extract derived from stingless bee Trigona thoracica in mice

  • Nurul Alina Muhamad Suhaini;Mohd Faeiz Pauzi;Siti Norazlina Juhari;Noor Azlina Abu Bakar;Jee Youn Moon
    • The Korean Journal of Pain
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    • v.37 no.2
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    • pp.141-150
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    • 2024
  • Background: Stingless bee propolis is a popular traditional folk medicine and has been employed since ancient times. This study aimed to evaluate the antinociceptive activities of the chemical constituents of aqueous propolis extract (APE) collected by Trigona thoracica in a nociceptive model in mice. Methods: The identification of chemical constituents of APE was performed using high-performance liquid chromatography (HPLC). Ninety-six male Swiss mice were administered APE (400 mg/kg, 1,000 mg/kg, and 2,000 mg/kg) before developing nociceptive pain models. Then, the antinociceptive properties of each APE dose were evaluated in acetic acid-induced abdominal constriction, hot plate test, and formalin-induced paw licking test. Administration of normal saline, acetylsalicylic acid (ASA, 100 mg/kg, orally), and morphine (5 mg/kg, intraperitoneally) were used for the experiments. Results: HPLC revealed that the APE from Trigona thoracica contained p-coumaric acid (R2 = 0.999) and caffeic acid (R2 = 0.998). Although all APE dosages showed inhibition of acetic acid-induced abdominal constriction, only 2,000 mg/kg was comparable to the result of ASA (68.7% vs. 73.3%, respectively). In the hot plate test, only 2,000 mg/kg of APE increased the latency time significantly compared to the control. In the formalin test, the durations of paw licking were significantly reduced at early and late phases in all APE groups with a decrease from 45.1% to 53.3%. Conclusions: APE from Trigona thoracica, containing p-coumaric acid and caffeic acid, exhibited antinociceptive effects, which supports its potential use in targeting the prevention or reversal of central and peripheral sensitization that may produce clinical pain conditions.

Determination of Sulfamethazine Residues in Urine, Kidney and Muscle of Slaughtered Pigs by SOS(sulfa on site) Test Kit and High - Performans Liquid Chromatography (SOS Test Kit 및 HPLC법에 의한 도축돈의 뇨, 신장 및 근육내 설파메타진 잔류량 조사)

  • 황인진;박병옥;김창수;우기방
    • Korean Journal of Veterinary Service
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    • v.13 no.1
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    • pp.21-26
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    • 1990
  • This survey was carried out to determine sulfamethazine residues in urine, kidney and muscle of slaughtered pigs. For this investigation, 20 samples for export and 30 samples for domestic market were collected at slaughterplant in Anyang city from the early of November to the end of December and comparatively were analyzed by SOS test kit and HPLC the results obtained were summarized as follows : 1. Five of 50 samples of swine urine which were inspected by SOS test kit were appeared to sulfamethazine positive 2. The sulfamethazine residue In one of 50 samples of swine muscle was exceeded 0.1ppm 3. The positive samples by SOS test kit were agreed with the results of HPLC quantitative analysis

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Antioxidative Substances in Mulberry Leaves (뽕잎(桑葉)에 함유된 항산화성 물질)

  • Shin, Doo-Ho
    • Journal of the Korean Applied Science and Technology
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    • v.15 no.3
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    • pp.27-31
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    • 1998
  • Antioxodative substances in Mulberry leaves were examined. Antioxidative substances in Mulberry leaves were extracted by 80% methanol agueous solution. Antioxidative activity of extract was determined by examining hydrogen donating ability on 1,1-diphenyl-2-picrylhydrazyl (DPPH) and the inhibitory effect on the formation of the peroxide from Linoleic acid in the test tube at $50^{\circ}C$. Antioxidative substance were, then, separated and indentified by thin layer chromatography(TLC), UV-Vis spectrum and High performance liquid chromatography(HPLC) methods. Hydrogen donating ability on DPPH and antioxidative ability on linoleic acid of the extracted antioxidative substance were higher than those of 100ppm butylated hydroxy toluene(BHT). The extracted antioxidative substances were separated by TLC using ethylacetate : chloroform : formic acid : water(8 : 1 : 1 : 1 v/v) as a solvent, and a spot at Rf=0.35 was detected. The spot was scraped from the plate, and extrated by methanol. The extract was analyzed by UV-Vis spetra and HPLC, and chlorogenic acid was identified as a antioxidative substance.