• Title/Summary/Keyword: high performance liquid chromatography

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Determination of cyromazine residues in agricultural commodities using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Cyromazine의 잔류분석법)

  • Song, Lee-Seul;Kim, Young-Hak;Lee, Su-Jin;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jung-Ah;Oh, Jae-Ho;Im, Moo-Hyeog;Chang, Woo-Suk;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.202-208
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    • 2012
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.

Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS (LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발)

  • Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.372-379
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    • 2007
  • A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

Nontuberculous Mycobacterial pulmonary Infection in Immunocompetent Patients (면역적격자에서 비결핵마이코박테리아의 폐감염)

  • Lee, Hyo-Won;Kim, Mi-Na;Shim, Tae-Sun;Bai, Gill-Han;Pai, Chik-Hyun
    • Tuberculosis and Respiratory Diseases
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    • v.53 no.2
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    • pp.173-182
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    • 2002
  • Background : Nontuberculous mycobacteria (NTM) have usually been considered to be contaminants of colonizers when isolated from respiratory specimens in Korea, where there is a high prevalence of tuberculosis and a low rate of HIV infections. Therefore, there has been few studies on the clinical significance of NTM species in immunocompetent patients were investigated. Methods : Thirty-five NTM isolates, for which species identification was requested by the treating physicians during 1999 at the Asan Medical Center, were retrospectively analyzed. They were identified to the species level by mycolic acid analysis using high-performance liquid chromatography. The medical records of the patients with the NTM isolates were reviewed to identify those patients who met the American Thoracic Society (ATS)'s criteria for mycobacterial pulmonary infection. Their antimicrobial susceptibility data were compared with the clinical outcomes. Results : The NTM were identified as M. intracellulare (6 isolates), M. avium (5), M. abscessus (5), M. gordonae (5), M. terrae complex (4), M. szulgai (2), M. kansasii (2), M. fortuitum (2), M. peregrinum (1), M. mucogenicum (1), M. celatum (1), and M. chelonae (1). All 35 patients showed clinical symptoms and signs of chronic lung disease, but none had a HIV infections; 16 (45.7%) patients were found to be compatible with a NTM pulmonary infection according to the ATS criteria, 5 and 4 cases were affected with M. intracellulare and M. abscessus, respectively; 8 patients had a history of pulmonary tuberculosis. 13 patients received antimycobacterial therapy for an average of 21 months and 9 patients were treated with second-line drugs. Only 4 patients had improved radiologically. Conclusion : A NTM should be considered a potential pathogen of pulmonary infections in immunocompetent patients with chronic pulmonary diseases. Most NTM infections were left untreated for a prolonged period and showed a poor outcome as a result, M. intracellulare and M. abscessus were the two most frequent causes of NTM pulmonary infections in this study. Species identification and antimycobacterial susceptibility tests based on the species are needed for the optimum management of a NTM pulmonary infection in patients.

Analysis of Antioxidant Activity and Serotonin Derivatives in Safflower (Carthamus tinctorius L.) Germplasm Collected from Five Countries (국외 수집 홍화 유전자원의 항산화 활성 및 세로토닌 유도체 함량 분석)

  • Jung, Yi Jin;Assefa, Awraris Derbie;Lee, Jae Eun;Lee, Ho Sun;Rhee, Ju Hee;Sung, Jung Sook
    • Korean Journal of Plant Resources
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    • v.32 no.5
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    • pp.423-432
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    • 2019
  • In order to select potential plant resources as functional materials and natural antioxidants, we evaluated antioxidant activity and serotonin derivatives of safflower germplasm collected from five countries. N-(p-Coumaroyl) serotonin (CS) and N-feruloylserotonin (FS) were analyzed by using Ultra Performance Liquid Chromatography (UPLC). Total polyphenol content (TPC) was determined by Folin-Ciocalteu method and antioxidant activities were estimated by 2,2-diphenyl-1-picryl-hydrazil (DPPH), 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) diammonium salt (ABTS), Ferric reducing antioxidant power (FRAP) and Reducing power (RP) assays. The TPC showed a range of 28.25 to $90.53{\mu}g$ gallic acid equivalent (GAE)/mg dried extract (DE). DPPH, ABTS, FRAP and RP assay were in the range of 18.76 to 93.98, 48.91 to 163.73, 3.80 to 132.29 and 26.32 to $80.08{\mu}g$ ascorbic acid equivalent (ASCE)/mg DE, respectively. Among the five countries, safflower seed collected from Iran had the highest levels of serotonin derivatives and antioxidant activities than other countries (p<0.05). CS showed high correlation with TPC, ABTS and DPPH (r=0.673,0.727,0.820), and FS showed high correlation with DPPH (r=0.740). Accessions IT321214 and IT321215 could be useful for development of new functional materials and could be used as a source of valuable natural antioxidant materials.

Production of Lignan-Rich Eggs as Functional Food by Supplementing Schisandra chinensis By-Product in Laying Hens (사료에 오미자 가공부산물 분말의 첨가 급여가 계란의 리그난 함량에 미치는 영향)

  • Hye Mi Kang;Eun Ji Park;Sun Young Park;Dae Youn Hwang;Jong-Choon Lee;Myunghoo Kim;Young Whan Choi
    • Journal of Life Science
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    • v.34 no.1
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    • pp.18-27
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    • 2024
  • Laying hens are known to be able to 'bio-accumulate' the health-promoting ingredients of their diet into eggs. The purpose of this study was to characterize lignan-rich eggs as functional food fed with Schisandra fruit by-product (SCP). Experimental diets were formulated using yellow corn, rice bran, soybean meal, fish meal, meat bone meal, poultry meal, vitamin premix, mineral premix, CaCO3, and supplemented Schisandra chinensis by-product. This experiment conducted a completely randomized design with 5 treatments for 5 laying hens. Levels of SCP were fed control diet or each formulated diet containing 1%, 3%, 5% and 7% SCP powder. The weight of eggs and the lignan content in white and yolk of egg were investigated every 7 days. Egg production and egg weight were not affected by diet at less than 5% SCP in the diet, but were significantly reduced when the diet was supplemented with a high concentration of 7% SCP after 3 weeks. Yolks and white in eggs were analyzed by using a high performance liquid chromatography (HPLC) to determine the lignans profile. Higher dietary SCP supplementation significantly increased gomisin N and schisandrin C in Acetonitrile (p<0.05). Gomisin N in egg white increased in a concentration-dependent manner, but shisandrin C not detected. These results indicated that the use of SCP powder in layering diets was effective in egg quality and for the production of lignans fortified eggs. In conclusion, dietary supplementation of Schisandra by-product with less than 5% can produce lignans-enrich eggs used as functional foods.

Study on the changes of sulfamethnzine residues in serum and practical organs of rats orally administrated with sulfamethnzine sodium (Rat에 sulfamethazine sodium 경구투여 후 혈청 및 실질장기내 sulfamethazine의 잔류량 추이에 관한 연구)

  • 도재철;이영미;조민희;신상희;박희주;송희종;정종식
    • Korean Journal of Veterinary Service
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    • v.23 no.4
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    • pp.321-333
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    • 2000
  • In order to know the depletive changes of sulfamethazine residues in senlm and practical organs of rats orally administered with sulfamethazine sodium(SMS), the concentration of sulfamethazine was measured in serum and tissue(kidney, liver, spleen, testis, and skeletal muscle) of rats with using high performance liquid chromatography(HPLC). SMS was orally administrated to sprague-dawley male rats(body weight, 200~300g) with using sonde at the rate of 20mg/100g body weight(recommended therapeutic dose) on once a day for 3 days. There were investigated the depletive changes of the sulfamethazine in serum, kidney, liver, spleen, testis and skeletal muscle of rat at the time 8 hours, 1st, 2nd, 3rd, 4th, 5th and 6th day after administration SMS, respectively. The results obtained were summarized as follows; 1. After oral administration of the SMS, the mean concentrations of sulfamethazine in serum according to the time lapsed were showed 215.53$\pm$42.99ppm at the 8 hours after withdrawal of medicated sulfamethazine. And gradually according to the time lapsed, the concentrations of sulfamethazine residues in serum were significantly (p<.05) decreased 25.87$\pm$5.18ppm at 1st day, 2.30$\pm$0.61ppm at 3rd day and 0.11$\pm$0.02ppm at 6th day respectively. 2. The mean concentrations of sulfamethazine in kidney, liver, spleen, muscle and testis according to the time lapsed after administration SMS were showed 83.82$\pm$12.16, 81.77$\pm$12.88, 36.96$\pm$5.35, 35.96$\pm$TEX>$\pm$1.39 and 27.89$\pm$1.92 ppm at the 8 hours, respectively. And gradually according to the time lapsed, the concentrations of sulfamethazine residues in the each of samples were significantly(p<.05) decreased such as 7.15$\pm$0.26, 5.62$\pm$0.72, 2.43$\pm$0.29, 1.99$\pm$0.14 and 3.11$\pm$0.48 ppm at 1st day, 0.52$\pm$0.04, 1.32$\pm$0.22, 0.13$\pm$0.03, 0.15$\pm$0.06 and 0.26$\pm$0.11ppm at 3rd day, and 0.03$\pm$0.01, 0.11$\pm$0.03, 0.02$\pm$0.01, 0.009$\pm$0.001 and 0.02$\pm$0.01 ppm at 6th day, respectively. 3. After oral administration of the SMS to rats, the residual concentrations of sulfamethazine in skeletal muscle were significantly (p<.05) decreased 35.96$\pm$1.39 to 0.009$\pm$$\pm$0.001 ppm between 8 hours and 6th day, respectively From the 4th day, the residual concentrations of sulfamethazine were showed 0.10$\pm$0.04 ppm below 0.1 ppm at the permitted limit concentration of muscle in Korea. In conclusion, this study could be suggested the relationship between administrated period, doses of sulfonamides and residual aspects of serum and practical organs, and the importance of observing ceasing period of antibiotic drugs before forwarding livestocks to slaughter.

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Isoflavone Contents in Some Varieties of Soybean and on Processing Conditions (콩의 종류와 가공 조건에 따른 isoflavone의 함량 변화)

  • 문보경;전기숙;황인경
    • Korean journal of food and cookery science
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    • v.12 no.4
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    • pp.527-534
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    • 1996
  • enistein (G), and daidzein (D), the major isoflavones, were analyzed in 14 varieties of Korean soybean and various processed soybean products by using high performance liquid chromatography. Isoflavone contents (G+D) were greatly variable among varieties ranged from 308.2 $\mu\textrm{g}$/g to 1,134.2 $\mu\textrm{g}$/g and highest in Danyopkong and Jinpumkong. Among hypocotyl, cotyledon and hull of soybean the concentration of the isoflavone (G+D) in the hypocotyl was highest ranged from 2,971.7 $\mu\textrm{g}$/g to 5,704.9 $\mu\textrm{g}$/g. The distributions of genistein and daidzein were also different in hypocotyl, cotyledon and hull. Higher ratio of daidzein to genistein (D/G) was found in the hypocotyl (4-12) compared to cotyledon and hull (0.1-4). Isoflavone (G+D) contents of soymilks (Sinpaldal#2, Eunhakong) prepared at 16 hour hydration were decreased to 1.1-1.2 times compared with that at 8 hour hydration. Commercial soymilks contained much lower isoflavone (G+D) than laboratory soymilks. Soybean curd (Eunhakong) prepared with MgCl$_2$ showed higher isoflavone (G+D) contents than that with CaSO$_4$. But these values of two different soybean curds made at laboratory were similar to those of 3 commercial curds. The concentration of the isoflavones in soybean sprout separated with 3 parts revealed highest in the head and lowest in the stem. Compared with non-fermented soybean foods the fermented soybean produfts, Kochujang and soybean paste, Duen Jang, showed very low contents of isoflavone (G+D),2.8-3.0 $\mu\textrm{g}$/g, 35.9-63.6 $\mu\textrm{g}$/grespectively.

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Fermentable Sugar Contents of Commercial Medical Foods and Carbohydrate Ingredients (상업용 메디컬푸드 및 탄수화물 급원의 발효성 당류 함량에 관한 연구)

  • Shin, Hee-Chang;Kang, Nam-Hee;Lee, Jang-Woon;Lee, Yoon-Bok;Lee, Kyun-Hee;Oh, Seung-Hyun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1200-1205
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    • 2015
  • Medical foods are enteral nutrition for patients, but they cause maladaptation symptoms like diarrhea. Although the cause of diarrhea remains unknown, some studies have indicated that the cause of diarrhea is fermentable oligosaccharides, disaccharides, monosaccharides, and polyols (FODMAP). This is a consideration for medical foods since they are easily fermented by intestinal bacterial. In this study, we estimated the FODMAP contents of commercial medical foods and carbohydrate ingredients. We measured the concentrations of FODMAP in 13 types of different medical foods and five types of carbohydrate ingredients by using high performance liquid chromatography with an evaporative light scattering detector (HPLC-ELSD). The limits of detection of FODMAP were fructose, 0.002; lactose, 0.010; raffinose, 0.003; stachyose, 0.032; 1-kestose, 0.005; nystose, 0.012; and 1-fructofuranosylnystose, 0.003 mg/kg. Limits of quantitation of FODMAP were fructose, 0.008; lactose, 0.033; raffinose, 0.009; stachyose, 0.107; 1-kestose, 0.015; nystose, 0.042; and 1-fructofuranosylnystose, 0.011 mg/kg, respectively. Concentration of FODMAP ranged from 0.428~2.968 g/200 mL. Concentrations of carbohydrate ingredients in FODMAP were chicory fiber, 278.423; soy fiber, 27.467; indigestible maltodextrin, 52.384; maltodextrin (DE10~15), 32.973; and maltodextrin (DE15~20), 50.043 g/kg. Contents of carbohydrates were 19.0~41.0 g/200 mL in commercial medical foods. We expected a correlation between contents of carbohydrates and FODMAP, as carbohydrates included FODMAP. However, we detected a low correlation (r=0.55). Since most commercial medical foods have a similar carbohydrate ingredients and nutritional values, the difference between products was determined by FODMAP contents of carbohydrate ingredients. In this study, we analyzed FODMAP contents of commercial medical foods and carbohydrate ingredients. These results are expected to be utilized as basic data for product development and minimizing maladaptation of medical foods.

Development and Validation of Analytical Method for Wogonin, Quercetin, and Quercetin-3-O-glucuronide in Extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus Mixture (연잎, 상엽, 건조 무 혼합 추출물의 지표성분 wogonin, quercetin 및 quercetin-3-O-glucuronide의 분석법 개발 및 검증)

  • Jang, Gill-Woong;Park, Eun-Young;Choi, Seung-Hyun;Choi, Sun-il;Cho, Bong-Yeon;Sim, Wan-Sup;Han, Xinggao;Cho, Hyun-Duk;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.289-295
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    • 2018
  • The aim of this study was to develop and validate an analytical method for determining the presence of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures. We evaluated the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of analytical methods for wogonin, quercetin, and quercetin-3-O-glucuronide using high performance liquid chromatography. Our result showed that the correlation coefficients of the calibration curve for wogonin, quercetin, and quercetin-3-O-glucuronide were 0.9999. The LOD for wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.09 to 0.16 and those for the LOQ ranged from 0.26 to $0.48{\mu}g/mL$. The inter-day and intra-day precision values of wogonin, quercetin, and quercetin-3-O-glucuronide ranged from 0.74 to 1.87 and from 0.28 to 1.12%, respectively. The inter-day and intra-day accuracies were 99.96~115.88% and 99.73~114.81%, respectively. Therefore, the analytical method was validated for the detection of wogonin, quercetin, and quercetin-3-O-glucuronide in extracts of Nelumbo nucifera, Morus alba L., and Raphanus sativus mixtures.

Protective effects of Gastrodia rhizoma and steamed & fermented Gastrodiae rhizoma with anti-oxidant efficacy and suppression of NFκB signaling pathway on LPS-induced liver injury (LPS로 유발한 간손상 마우스에서 항산화 및 항염증 효능을 통한 천마와 증숙 발효 천마의 간보호 효과)

  • Kim, Hyoung-Jin;Kwon, O Jun;Lee, Ah Reum;Roh, Seong-Soo;Seo, Young-Bae
    • Journal of Applied Biological Chemistry
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    • v.59 no.3
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    • pp.179-188
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    • 2016
  • This study is aimed to evaluate the protective effect of Gastrodiae rhizoma and steamed, dried & fermented Gastrodiae rhizoma on Lipopolysaccharide (LPS)-induced hepatic injury in the mice model. Sample was selected to GR0F0 (not processed gastrodia rhizome) and GR6F4 (fermented with Saccharomyces cerevisiae before steamed and dried 6 times) based on 1,1-diphenyl-2-picrylhydrazyl, 2,2'-azinobis-3-ethyl-benzothiazoline-6-sulfonic acid, and High-performance liquid chromatography analysis. Mice were randomly divided into 4 groups - Normal group, vehicle group (LPS treated), GR0F0 group (fed GR0F0 before LPS treated) and GR6F4 group (fed GR6F4 before LPS treated) with 6 mice in each group. GR0F0 group and GR6F4 group were fed each extract 200 mg/kg/day during 8 days. LPS 20 mg/kg injected to the experimental groups as abdominal injection. We measured aspartate aminotransferase, alanine amino-transferase in serum. GR0F0 and GR6F4 showed a significant decrease compared to the vehicle group. As a result of measuring the ROS, GR6F4 group showed a significant reduction in both the serum and liver tissues compared to the vehicle group. GR0F0 group showed a significant reduction only in the liver tissues. Activator protein-1, cyclooxygenase-2, and Inducible nitric oxide synthase were significantly decreased GR0F0 group and GR6F4 group. But tumor necrosis factor alpha only showed a significant reduction in GR6F4 group. GR0F0 and GR6F4 groups against liver damage in mice with LPS. That showed significant effects on anti-oxidant and anti-inflammatory action. The effects of GR6F4 group showed superior results compared to GR0F0 group. Therefore, Steamed, dried & fermented Gastrodia rhizoma was might have a protective effect on liver injury.