• Title/Summary/Keyword: liquid limits

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Determination of Analytical Method for the Insecticide Clothianidin and its Metabolites in Soil and Surface Water (토양 및 토양수 중 살충제 Clothianidin 및 대사산물 잔류분석법 확립)

  • Choi, Young-Joon;Kwon, Chan-Hyeok;Han, Byung-Soo;Lee, Young-Deuk
    • Korean Journal of Environmental Agriculture
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    • v.33 no.2
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    • pp.69-77
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    • 2014
  • BACKGROUND: The purpose of this study was to investigate the effects of clothianidin on the soil in terms of clothianidin dissipation and degradation to evaluate its safety in order to provide an analytical foundation for clothianidin and the 5 metabolites related to it. METHODS AND RESULTS: High-performance liquid chromatography(HPLC) was used to separate clothianidin and its metabolites in this study. In soil, after suppressing dissociation-proned ions with weak alkalic $NH_4OH$ and extracting the metabolites with methanol, clothianidin, Methylaminoimidazole(MAI), Methylnitroguanidine(MNG), Thiazolylmethylurea(TZMU) and Thiazolylnitroguanidine(TZNG). Thiazolylmethylguanidine(TMG) were extracted with the addition of neutral $NH_4OAC$ to increasing the intensity of ions. Compounding elements were separated by using Hydrometrix ($ChemElut^{TM}$) and ion-exchanging Solid-phase extraction(SPE) Strong cation-exchanger(SCX) and C18 were used. The recovery rates of clothianidin and 5 metabolites in soil and water ranged from 87.4% to 104.3%. A standard deviation of our analysis for the soil and water samples were less than 5%. CONCLUSION: Well accepted detection limits for clothianidin and 5 metabolites in soil samples based on a dissipation analysis is 0.005 mg/kg and 0.001 mg/L in water samples. The dissipation concentration of this study was decided to be enough to evaluate the dissipation levels of clothianidin and its metabolites.

Characteristics of Asphalt Concrete using Waste Foundry Sand (주물고사 첨가 아스팔트 콘크리트의 특성에 관한 연구)

  • Kim, Kwang-Woo;Ko, Dong-Hyuk;Choi, Dong-Chon;Kim, Sung-Won;Kim, Joong-Yul
    • International Journal of Highway Engineering
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    • v.3 no.4 s.10
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    • pp.105-116
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    • 2001
  • This study was performed to evaluate the characteristics of waste foundry sand (WFS) and the asphalt mixture made of a foundry waste sand. To estimate the applicability of WFS, chemical and physical properties were measured by XRF(X-ray fluorescent), and SEM(Scanning electronic microfilm). To improve the stripping resistance of WFS asphalt mixture, anti-stripping agents (a hydrated lime and a liquid anti-stripping agent) were used. To improve tensile properties and durability of WFS asphalt concrete mixture, LDPE(low-density polyethylene) was used as an asphalt modifier Marshall mix design, indirect tensile strength, tensile strength ratio(TSR) after freezing and thawing, moisture susceptibility and wheel tracking tests were carried out to evaluate performance of WFS asphalt concrete. Comparing with conventional asphalt concrete, WFS asphalt concretes showed similar or the better qualify in mechanical properties, and satisfied all specification limits. Therefore, it Is concluded that waste foundry sand can be recycled as an asphalt pavement material.

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Development and Application of a Method for Rapid and Simultaneous Determination of Three β-agonists (Clenbuterol, Ractopamine, and Zilpaterol) using Liquid Chromatography-tandem Mass Spectrometry

  • Sung, In Kyung;Park, Seo Jung;Kang, Kyutae;Kim, Min Young;Cho, Seongbeom
    • Food Science of Animal Resources
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    • v.35 no.1
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    • pp.121-129
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    • 2015
  • ${\beta}$-agonists are anabolic compounds that promote fat loss and muscle gain, and their administration to livestock may provide economic benefits by increasing growth rate and feed efficiency. For these reasons, ${\beta}$-agonists are also commonly added to livestock feed as growth promoters. This can introduce a significant risk of secondary human poisoning through intake of contaminated meat. A new method for the simultaneous determination of three ${\beta}$-agonists (clenbuterol, ractopamine, and zilpaterol) was developed in this study and applied to various meat samples. The limits of quantification, derived through a validation test following Codex guidelines, were $0.2{\mu}g/kg$ for clenbuterol and zilpaterol, and $0.4{\mu}g/kg$ for ractopamine. The average recoveries for clenbuterol, ractopamine, and zilpaterol ranged from 109.1% to 118.3%, 95.3% to 109.0%, and 94.1% to 120.0%, respectively. The recovery and coefficient of variation (CV) values fell within the acceptable range according to the Codex guidelines. This method reduced the analysis time without decreasing detection efficiency by modifying the pretreatment steps. This method could be utilized to manage the safety of imported meat products from countries where zilpaterol use is still permitted, thereby improving public health and preventing ${\beta}$-agonist poisoning due to secondary contamination.

Quality Evaluation of Five Commercial Enzyme Linked Immunosorbent Assay Kits for Detecting Aflatoxin B1 in Feedstuffs

  • Sun, Dan-Dan;Gu, Xu;Li, Jun-Guo;Yao, Ting;Dong, Ying-Chao
    • Asian-Australasian Journal of Animal Sciences
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    • v.28 no.5
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    • pp.691-696
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    • 2015
  • The objective of this study was to evaluate the quality of five commercial enzyme linked immunosorbent assay (ELISA) kits (A, B, C, D, and E) from different suppliers for detecting aflatoxin $B_1$ ($AFB_1$). $AFB_1$-free corn samples supplemented with different levels of $AFB_1$ (5, 10, and $20{\mu}g/kg$) were used as positive controls and 6 replicates of each control sample were tested to evaluate the accuracy and precision of these kits. In addition, we also evaluated the performance of these ELISA kits for $AFB_1$ in 30 feed samples, including corn, distillers dried grains with soluble, wheat samples, soybean meal, and poultry feed, which were verified by high performance liquid chromatography. Results showed that the coefficients of variation ranged from 1.18% to 16.22% in intra-plate and 2.85% to 18.04% in inter-plate for the determination of $AFB_1$. The half maximal inhibitory concentration for five kits ranged from 3.72 to $7.22{\mu}g/kg$. The quantitation limits of $AFB_1$ were all under the legal limit in China but somewhat inconsistent with kit instructions. Although the recovery rate of four of the five kits were either less than 90% or more than 110%, all these values were acceptable in practice. Two kits had high false positive rates (C and E). In conclusion, our results revealed that the qualities of five tested ELISA kits were significantly different.

Comparison of Analytical Methods for the Detection of Paralytic Shellfish Toxins (PSTs) (마비성패류독소 검출을 위한 분석법 비교)

  • Lee, Ka Jeong;Kwon, Soon Jae;Jung, Yeoun Joong;Son, Kwang Tae;Ha, Kwang Soo;Mok, Jong Soo;Kim, Ji Hoe
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.50 no.6
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    • pp.669-674
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    • 2017
  • Paralytic shellfish toxins (PSTs) are produced by marine dinoflagellate phytoplankton Alexandrium spp. and Gymnodinium spp. These toxins accumulate in filter feeding organisms such as bivalves and the ingestion of contaminated shellfish can cause illness in humans. The mouse bioassay (MBA) has been the preferred PST testing method worldwide for more than 50 years. However, this assay has several disadvantages, such as detection limits, non-toxic-profiles, and the ethical issues of using animals. The aim of this study was to establish an alternative to the MBA method for testing for PSTs. We optimized the analysis conditions of a post-column oxidation-high performance liquid chromatography (PCOX-HPLC) method and the Scotia Rapid Test Kit, and then compared the accuracy of these methods to the MBA method. The results demonstrated a strong correlation between the PCOX-HPLC method and the MBA, although the PCOX-HPLC method required expensive equipment and standard material, and was time consuming. The Scotia Rapid Test Kit promises to be a useful tool, as it provided rapid and qualitative results, although the method sometimes gave a false positive result that could not be explained by toxin profiles.

Quantitative Determination of the Bioactive Marker Components in Gyeji-tang Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 계지탕 중 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.49 no.1
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    • pp.76-83
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    • 2018
  • A traditional herbal formula, Gyeji-tang has been used to treat the early colds, headache, chills, and fever in Asian countries. In this study, we were performed simultaneous determination of the 14 bioactive marker compounds, gallic acid, spinosin, paeoniflorin, albiflorin, liquiritin apioside, liquiritin, 6'''-feruloylspinosin, liquilitigenin, coumarin, cinnmamic acid, benzoylpaeoniflorin, cinnamaldehyde, glycyrrhizin, and 6-gingerol in Gyeji-tang using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS). Analytical column was used a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) and maintained at $45^{\circ}C$ with a flow rate of 0.3 mL/min. The mobile phase consists of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was conducted using multiple reaction monitoring in the positive and negative modes by a Waters ACQUITY TQD LC-MS/MS system. The calibration curves of 14 bioactive marker compounds showed linearity with correlation coefficients ${\geq}0.9798$. The limits of detection and quantification values were in the range of 0.11-6.66 ng/mL and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the established LC-MS/MS method, the amounts of tested 14 compounds in the lyophilized Gyeji-tang sample were detected up to $85.7{\mu}g/g$. These results may be useful for quality assessment of a traditional herbal formulas.

Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

Bioequivalence Assessment of Roxithromycin Tablets in Healthy Korean Volunteers

  • Kwon Oh-Seung;Kim Hye-Jung;Pyo Hee-Soo;Chung Youn-Bok
    • Biomolecules & Therapeutics
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    • v.14 no.1
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    • pp.50-55
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    • 2006
  • The objective of the study was to evaluate the bioequivalency between the $Rozid^{TM}$ Tablet (Ilhwa Pharm. Co., Ltd.) as a test formulation and the $Rulid^{TM}$ Tablet (Handok Pharm. Co., Ltd) as a reference formulation. Twenty-four healthy male volunteers were administered the formulations by the randomized Latin square crossover design, and the plasma samples were determined by a high performance liquid chromatography (HPLC) with fluorescence detector. $AUC_t,\;C_{max}\;and\;T_{max}$ were obtained from the time-plasma concentration curves, and log-transformed $AUC_t\;and\;C_{max}$ and log-untransformed $T_{max}$ values for two formulations were compared by statistical tests and analysis of variation. $AUC_t$ was determined to be $63.30{\pm}25.57{\mu}g.hr/ml$ for the test formulation and $64.02{\pm}29.27mg.hr/ml$ for the reference formulation. The mean values of $C_{max}$ for the test and reference formulations were $5.07{\pm}2.14\;and\;5.53{\pm}2.60{\mu}g/ml$, respectively. The $AUC_t,\;and\;C_{max}$ ratios of the test $Rozid^{TM}$ Tablet to the reference $Rulid^{TM}$ Tablet were -1.12% and -8.32%, respectively, showing that the mean differences were satisfied the acceptance criteria within 20%. The results from analysis of variance for log-transformed $AUC_t,\;and\;C_{max}$ indicated that sequence effects between groups were not exerted and 90% confidence limits of the mean differences for $AUC_t,\;and\;C_{max}$ were located in ranges from log 0.80 and log 1.25, satisfying the acceptance criteria of the KFDA bioequivalence. The RozidTM Tablet as the test formulation was considered to be bioequivalent to the RulidTM Tablet used as its reference formulation, based on $AUC_t,\;and\;C_{max}$ values.

Establishment of an Analytical Method of Fluoroquinolones in Milk by HPLC (HPLC를 이용한 우유에서의 fluoroquinolones 시험법 확립)

  • Kim, Jong-Hwa;Hong, Se-Lyung;Kang, Tae-Beom;Lee, Hyun-Kyung;Lee, Soon-Ho
    • Korean Journal of Food Science and Technology
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    • v.42 no.5
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    • pp.521-526
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    • 2010
  • A high-performance liquid chromatography (HPLC) method was established for the determination of fluoroquinolones in milk. Protein was removed by using trichloroacetic acid in order to increase a mean recovery of milk. The extracts were using $Strata^{TM}$-X solid-phase extraction cartridge. The analytes were detected by HPLC on a $C_{18}$ column. HPLC method with fluorescence detection system (Ex: 278 nm, Em: 456 nm) provided a high degree of sensitivity in detecting fluoroquinolones. The limits of quantitation (LOQ) and mean recoveries of fluoroquinolones were 40 ${\mu}g$/kg and 73.6-95.2% (ofloxacin), 10 ${\mu}g$/kg and 77.3-91.9% (norfloxacin), 20 ${\mu}g$/kg and 91.6-94.3% (ciprofloxacin), 10 ${\mu}g$/kg and 81.0-87.8% (enrofloxacin), 10 ${\mu}g$/kg and 71.3-81.0% (sarafloxacin), 10 ${\mu}g$/kg and 89.4-90.8% (orbifloxacin), 2 ${\mu}g$/kg and 69.4-85.5% (danofloxacin).

Monitoring and Risk Assessment of Pesticide Residues in Commercially Dried Vegetables

  • Seo, Young-Ho;Cho, Tae-Hee;Hong, Chae-Kyu;Kim, Mi-Sun;Cho, Sung-Ja;Park, Won-Hee;Hwang, In-Sook;Kim, Moo-Sang
    • Preventive Nutrition and Food Science
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    • v.18 no.2
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    • pp.145-149
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    • 2013
  • We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography- ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended.