• Title/Summary/Keyword: Detection limits

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Simultaneous Determination of Vitamin A and E in Infant Formula by HPLC with Photodiode Array Detection

  • Lee, Hong-Min;Kwak, Byung-Man;Ahn, Jang-Hyuk;Jeong, Seung-Hwan;Shim, Sung-Lye;Kim, Kyong-Su;Yoon, Tae-Hyung;Leem, Dong-Gil;Jeong, Ja-Young
    • Food Science of Animal Resources
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    • v.31 no.2
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    • pp.191-199
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    • 2011
  • The objective of this study was to develop a method to simultaneously quantify vitamins A and E in infant formula. To determine the vitamin A and E content, vitamin A and four different vitamin E isomers (${\alpha}$-, ${\beta}$-, ${\gamma}$-, and ${\delta}$-tocopherol) were separated by high performance liquid chromatography with a photodiode array detector using a Develosil RPAQUEOUS RP-$C_{30}$ column ($4.6{\times}250$ mm, 5 ${\mu}M$). The vitamin A and E contents in the certified reference material determined using this method were within the certified range of standard values. The limits of detection (LODs) and limits of quantitation (LOQs) for vitamin A were 0.02 and 0.06 ${\mu}g/L$, respectively. LODs and LOQs for the vitamin E isomers ranged from 0.20 to 0.55 and from 0.67 to 1.81 ${\mu}g/L$, respectively. Linear analyses indicated that the square of the correlation coefficient for the vitamin A and E isomers was 0.9997-0.9999. The recovery of vitamins ranged from 96.69 to 97.79%. The results demonstrate that this novel method could be used to reliably analyze vitamin A and E content in infant formula.

Comparison between the liquid-liquid partition method and modified QuEChERS method for the analysis of pesticide residues in beef fat (소지방 중 잔류농약분석을 위한 액-액분배법과 modified QuEChERS법 비교)

  • Kim, Yoen-Joo;Choi, Yoon-Hwa;Shin, Bang-Woo;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.34 no.4
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    • pp.429-439
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    • 2011
  • This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

A study on characteristics of influent and effluent pollutants in public sewage treatment works combined with industrial wastewater and landfill leachate (공공하수처리시설에서 수질오염물질 유입 및 배출 특성 고찰 - 산업폐수 및 매립지 침출수 연계처리 시설을 중심으로 -)

  • Jeong, Dong-Hwan;Cho, Yangseok;Ahn, Kyung-Hee;Kim, Eunseok;Kim, Changsoo;Chung, Hyen-Mi
    • Journal of Korean Society of Water and Wastewater
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    • v.30 no.6
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    • pp.673-682
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    • 2016
  • In this study, we investigated influent and effluent water pollutants in 53 Public Sewage Treatment Works (PSTWs) where industrial wastewater or landfill leachate is combined four times for two years from 2014 to 2015. Also, we analyzed the characteristics of heavy metals and volatile organic carbons at influent and effluent of these PSTWs caused by sewage treatment combined with industrial wastewater or landfill leachate. As a result, six heavy metals such as barium, copper, iron, manganese, nickel and zinc, and four volatile organic carbons (VOCs) including phenols, di(2-)ethylhexyl phthalate (DEHP), formaldehyde and toluene were observed above detection limits in most of PSTWs. Also, it was revealed that six heavy metals such as hexavalent chromium, mercury, cadmium, chromium, nickel and selenium, and four VOCs including 1,1-dichloroethylene, vinyl chloride, naphthalene, and epichlorohydrin were observed more frequently according to precipitation. As a result of reviewing the monitoring data on "Water Quality Monitoring Networks" in lower watersheds of PSTWs, both heavy metals and VOCs were below detection limits, indicating that the effluent water had little influence on the watershed. Nevertheless for the better management of influent and effluent pollutants in PSTWs, it is necessary to establish the advanced management plans for water pollutants in PSTWs, which include a list of priority substances management, monitoring plans, and guidelines for industrial wastewater and landfill leachate combined in PSTWs.

Development of an analytical method for the determination of dl-methylephedrine hydrochloride in porcine muscle using liquid chromatography-tandem mass spectrometry (LC-MS/MS를 이용한 돼지 근육조직 중 dl-methylephedrine hydrochloride의 잔류 분석법 개발)

  • Chae, Won-Seok;Kim, Suk;Lee, Hu-Jang
    • Korean Journal of Veterinary Research
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    • v.60 no.4
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    • pp.209-213
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    • 2020
  • This study examined the residue of dl-methylephedrine hydrochloride (MEP) on the muscle of pigs administered orally with MEP 12 g/ton feed for seven consecutive days. Twenty healthy cross swine were administered MEP. Four treated animals were selected arbitrarily to be sacrificed at 1, 2, 3, 4, and 5 days after treatment. MEP residue concentrations in the muscle were determined by liquid chromatography coupled with tandem mass spectrometry. The drug was extracted from muscle samples using 10 mM ammonium formate in acetonitrile followed by clean-up with n-hexane. The analyte was separated on an XBridgeTM hydrophilic interaction liquid chromatography column using 10 mM ammonium formate in deionized distilled water and acetonitrile. The correlation coefficient (R2) of the calibration curve was 0.9974, and the limits of detection and quantification were 0.05 and 0.15 ㎍/kg, respectively. The recoveries at three spiking levels were 94.5-101.2%, and the relative Standard Deviations was less than 4.06%. In the MEP-treated group, MEP residues on one day post-treatment were below the maximum residue limit in the muscle. The developed method is sensitive and reliable for the detection of MEP in porcine muscle tissues. Furthermore, it exhibits low quantification limits for animal-derived food products destined for human consumption.

Development of reverse transcription loop-mediated isothermal amplification assays for point-of-care testing of avian influenza virus subtype H5 and H9

  • Zhang, Songzi;Shin, Juyoun;Shin, Sun;Chung, Yeun-Jun
    • Genomics & Informatics
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    • v.18 no.4
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    • pp.40.1-40.8
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    • 2020
  • Avian influenza (AIV) outbreaks can induce fatal human pulmonary infections in addition to economic losses to the poultry industry. In this study, we aimed to develop a rapid and sensitive point-of-care AIV test using loop-mediated isothermal amplification (LAMP) technology. We designed three sets of reverse transcription LAMP (RT-LAMP) primers targeting the matrix (M) and hemagglutinin (HA) genes of the H5 and H9 subtypes. RT-LAMP targeting the universal M gene was designed to screen for the presence of AIV and RT-LAMP assays targeting H5-HA and H9-HA were designed to discriminate between the H5 and H9 subtypes. All three RT-LAMP assays showed specific amplification results without nonspecific reactions. In terms of sensitivity, the detection limits of our RT-LAMP assays were 100 to 1,000 RNA copies per reaction, which were 10 times more sensitive than the detection limits of the reference reverse-transcription polymerase chain reaction (RT-PCR) (1,000 to 10,000 RNA copies per reaction). The reaction time of our RT-LAMP assays was less than 30 min, which was approximately four times quicker than that of conventional RT-PCR. Altogether, these assays successfully detected the existence of AIV and discriminated between the H5 or H9 subtypes with higher sensitivity and less time than the conventional RT-PCR assay.

Development of a Laser Absorption NO/$NO_2$ Measuring System for Gas Turbine Exhaust Jets

  • Zhu, Y.;Yamada, H.;Hayashi, S.
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2004.03a
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    • pp.802-806
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    • 2004
  • For the protection of the local air quality and the global atmosphere, the emissions of trace species including nitric oxides (NO and NO$_2$) from gas turbines are regulated by local governments and by the International Civil Aviation Organization. In-situ measurements of such species are needed not only for the development of advanced low-emission combustion concepts but also for providing emissions data required for the sound assessment of the effects of the emissions on environment. We have been developing a laser absorption system that has a capability of simultaneous determination of NO and NO$_2$concentrations in the exhaust jets from aero gas turbines. A diode laser operating near 1.8 micrometer is used for the detection of NO while a separated visible tunable diode laser operating near 676 nanometers is used for NO$_2$. The sensitivities at elevated temperature conditions were determined for simulated gas mixtures heated up to 500K in a heated cell of a straight 0.5 m optical path. Sensitivity limits estimated as were 30 ppmv-m and 3.7 ppmv-m for NO and NO$_2$, respectively, at a typical exhaust gas temperature of 800K. Experiments using the simulated exhaust flows have proven that $CO_2$ and $H_2O$ vapor - both major combustion products - do not show any interference in the NO or NO$_2$ measurements. The measurement system has been applied to the NO/NO$_2$ measurements in NO and NO$_2$ doped real combustion gas jets issuing from a rectangular nozzle having 0.4 m optical path. The lower detection limits of the system were considerably decreased by using a multipass optical cell. A pair of off-axis parabola mirrors successfully suppressed the beam steering in the combustion gas jets by centralizing the fluctuating beam in sensor area of the detectors.

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Establishment of withdrawal time and analysis of tiamulin residue in tissues of orally dosed broiler chickens (육계의 조직 중 티아물린의 잔류 분석 및 휴약기간 설정 연구)

  • Woo H. Kim;Jun Young Kim;Kwang Il Park;Yeung Bae Jin;Suk Kim;Hu-Jang Lee
    • Korean Journal of Veterinary Research
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    • v.63 no.3
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    • pp.23.1-23.9
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    • 2023
  • This study was conducted to investigate tiamulin (TML) residues in the edible tissues of orally dosed broiler chickens and to re-establish the withdrawal time (WT). Thirty-six healthy Ross broiler chickens were administered 0.5 (TML-1) and 2.5 kg (TML-2) per ton feed, respectively, of the drug containing TML 78 g/kg for 10 days. Twenty-four tissue samples were collected from 6 chickens in each of the TML-1 and TML-2 groups on 0, 1, 3, and 5 days after drug administration, respectively. The residual concentrations of TML were measured using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The correlation coefficient of the calibration curves was 0.9978 to 0.9998, and the limits of detection and the limits of quantification (LOQ) were in the range of 0.03 to 0.06, and 0.1 to 0.2 ㎍/kg, respectively. Recoveries ranged between 89.0% to 116.7%, and the coefficients of variation were less than 13.9%. After the drug administration, TML in the TML-1 and TML-2 groups was detected above the LOQ in 1 and 6 samples of liver, respectively, at day 0, and in 1 liver sample from both groups on day one. At 3 days after administration, TML was detected below the LOQ in all samples of TML-1 and TML-2. The calculated WT of TML in both TML-1 and TML-2 using the WT calculation program WT 1.4 was 0 days. In conclusion, the developed analytical method is suitable for detection, and the calculated WT of TML in poultry edible tissues is shorter than the current recommended WT of 7 days for TML in broiler chickens.

Analysis of tetracyclines in shrimp samples based on a two-step extraction approach prior to high-performance liquid chromatography

  • Thinnakorn Sukkhunthod;Thanakorn Pluangklang;Sumita Boonnab;Sira Sansuk;Phitchan Sricharoen;Maliwan Subsadsana
    • Analytical Science and Technology
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    • v.37 no.4
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    • pp.211-219
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    • 2024
  • This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R2 > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

Conventional Analytical and New Raman Spectroscopy-Based Methods for Detecting Benzo[a]pyrene in Food: Review and Perspective (식품 내 벤조피렌 분석법의 기존 연구동향 및 라만분광법 기반기술 전망)

  • Lee, Mi-Hyun;Yee, So-Yoon;Jin, Xuanyan;Choi, Dae Sik;Rhee, Hanju;Rhee, Jin-Kyu
    • Microbiology and Biotechnology Letters
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    • v.43 no.3
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    • pp.177-186
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    • 2015
  • With a view to supporting the provisions of the current Korean food code for the detection of Benzo[a]pyrene, various analytical methods of detection in foods were evaluated and established in terms of linearity, limits of detection/quantitation, efficiency, and accuracy, amongst others. It was observed that to improve the technologies involved in the application of these methods, complicated and combined preparation processes of foods, including extraction, separation and purification, have been the main focus of efforts at optimization. Recently, on-site quick reaction for the detection of hazardous substances in the environment and food materials aims at developing simplified examination processes, such as lable-free and non-invasive technological analysis, to reduce the costs and time involved in the examination. Herein, current benzo[a]pyrene detection methods are reviewed in addition to new Raman spectroscopy-based trials established to pursue improve the speed, simplicity and suitability of testing.

Direct Identification of Vibrio vulnificus by PCR Targeting Elastase Gene

  • Lee, Jae-Won;Jun, In-Joon;Kwun, Hyun-Jin;Jang, Kyung-Lib;Cha, Jae-Ho
    • Journal of Microbiology and Biotechnology
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    • v.14 no.2
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    • pp.284-289
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    • 2004
  • A PCR assay for the rapid detection of Vibrio vulnificus strains was developed using a virulence gene for elastase found in various Vibrio species. The DNA sequences in the elastase gene facilitated the identification of a species-specific probe for pathogenic V. vulnificus strains from both clinical and environmental sources. Using an elastase gene-based PCR reaction, a species-specific 507-bp PCR product was visualized by agarose gel electrophoresis. Three different DNA extraction methods were then compared to improve the simplicity and rapidity of detection. A PCR assay using the conventional DNA extraction or boiling method was able to detect as few as 25 V. vulnificus cells, making the detection limits at least 1-log-scale lower than that for the EDT A-treated DNA extraction method. In particular, the boiling method, which does not require purification of the chromosomal DNA, was very effective in terms of simple and rapid detection. Meanwhile, the detection limit in a mixed bacterial culture that included other bacteria, such as Escherichia coli or Bacillus subtilis, was two V. vulnificus cells, which was 1-log-scale lower than that for the control. Accordingly, when coupled with a new DNA extraction method, the elastase gene-based PCR can provide a rapid, specific, and sensitive method for identifying V. vulnificus in clinical and environmental samples.