• Title/Summary/Keyword: method detection limit

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Gas Chromatographic Performances for Simultaneous Determination of Multi-pesticide Residues and Extraction of Pesticides with Three Partition Solvents (잔류농약 다성분 동시분석을 위한 기체 크로마토그래피 분석성능과 3종 분배용매에 의한 농약추출)

  • Kim, Chan-Sub;Kim, Jin-Bae;Im, Geon-Jae;Park, Hyun-Ju;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.13 no.3
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    • pp.133-147
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    • 2009
  • In order to develop the simultaneous analytical method for pesticide residues which ones in soil are rapidly and inexpensively measured by, many analytical methods for individual pesticide residue and several methods for multi-pesticide residues in agricultural commodities and food were reviewed. Various gas chromatographic conditions and pre-treatment procedures were intensively investigated and modified. And then new optimum procedure was established and its proficiency was validated. The response on detectors of simultaneous determination of 180 pesticides out of pesticides used in Korea was tested. The number of pesticides that their limits of detection (LOD) equal or lower than $0.05\;mg\;kg^{-1}$ were 137 pesticides on ECD, 170 pesticides on NPD and 179 pesticides on ECD/NPD integrated. The retention times of most pesticides ranged appropriately between 10 minutes and 40 minutes in the proposed chromatographic conditions. But about 90 pesticides eluded between 20 minutes and 30 minutes and so they were not resolved enough. In partition with dichloromethane, ethyl acetate/hexane (1:1) and ethyl acetate, number of pesticides whose extraction efficiency ranged from 70% to 120%, were 163, 154 and 147, respectively.

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.

Refined Exposure Assessment for Three Active Ingredients of Humidifier Disinfectants

  • Lee, Jong-Hyeon;Kang, Hyun-Joong;Seol, Hwi-Soo;Kim, Chan-Kook;Yoon, Seung-Ki;Gwack, Jin;Kim, Yong-Hwa;Kwon, Jung-Hwan
    • Environmental Engineering Research
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    • v.18 no.4
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    • pp.253-257
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    • 2013
  • Exposure assessment for three major active ingredients used for humidifier disinfectants, polyhexamethylene guanidine (PHMG), oligo(2-(2-ethoxy)ethoxyethyl guanidinium chloride (PGH), and 5-chloro-2-methylisothiazol-3(2H)-one/2-methylisothiazol-3(2H)-one (CMIT/MIT) mixture, was conducted in a bedroom using an air sampler for a refined risk assessment. The experimental site was selected to reflect consumer exposure conditions. Aerosols formed by a humidifier were sampled during 8 hr at 7.5 L/min. Absorbed PHMG and PGH by the sampler were quantified using a spectrophotometric method, and high performance liquid chromatography-ultraviolet detection was used for CMIT/MIT. Three exposure scenarios were assumed for adding humidifier disinfectants to the humidifier water at 1, 2, and 10 times the volume recommended by the product suppliers, and the humidifier was on at its maximum rate of producing aerosols in order to consider reasonable worst-cases. The sampled mass of PHMG and PGH ranged 200 to $2,800{\mu}g$ and 140 to $1,900{\mu}g$, respectively, under different exposure conditions, whereas the absorbed mass of CMIT/MIT was barely detected at the detection limit of 0.11/0.29 mg/L, only at 10 times the recommended level. The resulting risk quotients for PHMG and PGH ranged 1,400 to 20,000 and 1,000 to 13,000, indicating that health risks could be significant. For CMIT/MIT mixture, risk quotients were much smaller than estimated by assuming that they are conservative in the indoor environment, probably due to oxidative reactions. The refined exposure assessment presented here may provide a useful tool for assessing risks posed by active ingredients in spray-type biocidal products.

ELISA Development for the residue of the organophosphorus insecticide acephate (ELISA에 의한 유기인계 살충제 Acephate 잔류물 분석법 개발)

  • Lee, Jae-Koo;Ahn, Ki-Chang;Stoutamire, Donald W.;Gee, Shirley J.;Hammock, Bruce D.
    • The Korean Journal of Pesticide Science
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    • v.5 no.2
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    • pp.1-12
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    • 2001
  • A competitive indirect enzyme-linked immunosorbent assay (ci ELISA) for the organophosphorus insecticide acephate, O,S-dimethyl acetylphosphoramidothioate, was developed using a polyclonal antibody. Three different haptens mimicking the analyze and containing hexanoic acid moiety as a linker were synthesized, and then conjugated with the carrier proteins bovine serum albumin and keyhole limpet hemocyanin by the N-hydroxysuccinimide active ester method. Polyclonal antibodies raised against hapten-KLH conjugates in rabbits and the hapten-BSA conjugates as coating antigens were screened and selected for the assay in the homologous and/or heterologous ELISA system. The effects of various assay conditions, including blocking reagents, detergent content, organic solvents, pH, and preincubation of tile mixture of the polyclonal antibody and the analyze on the sensitivity were evaluated. The $IC_{50}$ value of acephate of 110 ng/mL was obtained in an optimized heterologous system using hapten-3-BSA as a coating antigen and a polyclonal antibody 8377, showing the detection range of 10-1000 ng/mL and the lowest detection limit of 4 ng/mL. The cross-reactivities of the structurally related insecticides, including methamidophos were less than 0.02%. These results indicate that the ELISA could be a convenient and alternative tool for monitoring acephate residues in agricultural products and environmental samples.

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Development of Disposable Immunosensors for Rapid Determination of Sildenafil and Vardenafil in Functional Foods

  • Vijayaraj, Kathiresan;Lee, Jun Hyuck;Kim, Hyung Sik;Chang, Seung-Cheol
    • Journal of Food Hygiene and Safety
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    • v.32 no.2
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    • pp.83-88
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    • 2017
  • We introduced disposable amperometric immunosensors for the detection of Sildenafil and Vardenafil (SDF/VDF) based on screen printed carbon electrodes. The developed immunosensors were used as a non-competitive sandwich-type enzyme immunoassay with a horseradish peroxidase label. The sensors were constructed on screen printed carbon electrodes by the simple electrochemical deposition of a reduced graphene oxide and chitosan (ErGO-CS) composite. To evaluate the sensing chemistry and optimize the sensor characteristics, a series of electrochemical experiments were carried out including electrochemical impedance spectroscopy, cyclic voltammetry and amperometry. The sensors showed a linear response to SDF/VDF concentrations in a range from 100 pg/mL to 300 ng/mL. The lower detection limit was calculated to be 55 pg/mL, the sensitivity was calculated to be $1.02{\mu}Ang/mL/cm^2$, and the sensor performance exhibited good reproducibility with a relative standard deviation (RSD) of 7.1%. The proposed sensing chemistry strategy and the sensor format can be used as a simple, cost-effective, and feasible method for the in-field analysis of SDF/VDF in functional or health supplement food samples.

A Method of Machine Learning-based Defective Health Functional Food Detection System for Efficient Inspection of Imported Food (효율적 수입식품 검사를 위한 머신러닝 기반 부적합 건강기능식품 탐지 방법)

  • Lee, Kyoungsu;Bak, Yerin;Shin, Yoonjong;Sohn, Kwonsang;Kwon, Ohbyung
    • Journal of Intelligence and Information Systems
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    • v.28 no.3
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    • pp.139-159
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    • 2022
  • As interest in health functional foods has increased since COVID-19, the importance of imported food safety inspections is growing. However, in contrast to the annual increase in imports of health functional foods, the budget and manpower required for inspections for import and export are reaching their limit. Hence, the purpose of this study is to propose a machine learning model that efficiently detects unsuitable food suitable for the characteristics of data possessed by government offices on imported food. First, the components of food import/export inspections data that affect the judgment of nonconformity were examined and derived variables were newly created. Second, in order to select features for the machine learning, class imbalance and nonlinearity were considered when performing exploratory analysis on imported food-related data. Third, we try to compare the performance and interpretability of each model by applying various machine learning techniques. In particular, the ensemble model was the best, and it was confirmed that the derived variables and models proposed in this study can be helpful to the system used in import/export inspections.

A Study on Public Awareness of Landslide and Check Dam Using the Big Data Platform 'Hyean' (공공 빅데이터 플랫폼 '혜안'을 통한 산사태 및 사방댐 인식 분석)

  • Sohee Park;Min Jeng Kang;Song Eu
    • Journal of the Society of Disaster Information
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    • v.18 no.4
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    • pp.687-698
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    • 2022
  • Purpose: This study was conducted to understand the public awareness of landslide and check dams in 2015-2020 using the big data platform 'Hyean' and to confirm the utilization of this platform in disaster prevention areas. Method: The total amount, number of detection by period by media, and affirmative and negative trends of a search for 'landslide' and 'check dam' in 2015-2020 were analyzed using a keyword search of 'Hyean.' Result: There is significant lack of public awareness of check dam compared to landslide, and the trend is more noticeable in the conspicuous gap of data amount between the news and SNS media. The number and the timing of the search for 'landslide' coincided with the actual occurrence of landslide, while the detection of 'check dam' was less related to it. Relatively affirmative preception for the check dam is inferred, but it was difficult to confirm accurate statistical affirmative and negative trends in the disaster prevention field using 'Hyean.' Conclusion: Unlike the experts who expect positive public awareness of check dam, the statistic results show that the public awareness of the check dam as an effective countermeasure against landslide was extremely low. Active promotion of erosion control projects should be carried out first, and a balanced sample survey should accompany online and periodic field surveys. Since there is a limit to grasping the effective perception in the field of disaster prevention area using 'Hyean', it should be very cautious to establish local/governmental policies using it.

Highly ordered In2O3 zig-zag nanocolumns for selective detection of acetone (아세톤의 선택적 감지를 위한 In2O3 zig-zag nanocolumns)

  • Jae Han Chung;Ho-Gyun Kim;Yun-Haeng Cho;Junho Hwang;See-Hyung Park;Sungwoo Sohn;Su Bin Jung;Eunsol Lee;Kwangjae Lee;Young-Seok Shim
    • Journal of the Korean institute of surface engineering
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    • v.57 no.1
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    • pp.38-48
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    • 2024
  • We fabricated In2O3 zig-zag nanocolumns(ZZNCs) by oblique angle deposition method based on e-beam evaporator for highly sensitive and selective CH3COCH3 sensor. Our results indicate that as the ZZNCs layer stacks, the gas response also increases. In comparison to thin films, ZZNCs at 5 layer show a 117-fold enhancement in gas response and a rapid response time (~2 s). When measured with various gases, it showed a high selectivity towards acetone. Under conditions of 80% R.H., exposure to CH3COCH3 gas theoretically indicated a detection limit of 1.2 part-per-billion(ppb). These results suggest the potential of In2O3 ZZNCs as a breath analyzer for the diagnosis of diabetes.

Simultaneous Determination of Penicillin Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 페니실린계 항생제 8종의 동시분석 및 적용성 검증)

  • Kim, Myeong-Ae;Yoon, Su-Jin;Kim, MeeKyung;Cho, Yoon-Jae;Choi, Sun-Ju;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.131-140
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    • 2014
  • The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).

Determination of Mycotoxins in Agricultural Products Used for Food and Medicine Using Liquid Chromatography Triple Quadrupole Mass Spectrometry and Their Risk Assessment (LC-MS/MS를 이용한 식·약 공용 농산물의 곰팡이독소 분석 및 위해평가)

  • Choi, Su-Jeong;Ko, Suk-Kyung;Park, Young-Ae;Jung, Sam-Ju;Choi, Eun-Jung;Kim, Hee-sun;Kim, Eun-Jung;Hwang, In-Sook;Shin, Gi-Young;Yu, In-Sil;Shin, Yong-Seung
    • Journal of Food Hygiene and Safety
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    • v.36 no.1
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    • pp.24-33
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    • 2021
  • For this study, we surveyed concentrations of 8 mycotoxins (aflatoxin B1, B2, G1, G2, ochratoxin A, fumonisin B1, B2 and zearalenone) in agricultural products used for food and medicine by liquid chromatography-tandem mass spectrometry and conducted a risk assessment. Samples were collected at the Yangnyeong Market in Seoul, Korea, between January and November 2019. Mycotoxins were extracted from these samples by adding 0.1% formic acid in 50% acetonitrile and cleaned up by using an ISOLUTE Myco cartridge. The method was validated by assessing its matrix effects, linearity, limit of detection (LOD), limit of quantification (LOQ), recovery and precision using four representative matrices. Matrix-matched standard calibration was used for quantification and the calibration curves of all analytes showed good linearity (r2>0.9999). LODs and LOQs were in the range of 0.02-0.11 ㎍/kg and 0.06-0.26 ㎍/kg, respectively. Sample recoveries were from 81.2 to 118.7% and relative standard deviations lower than 8.90%. The method developed in this study was applied to analyze a total of 187 samples, and aflatoxin B1 was detected at the range of 1.18-7.29 ㎍/kg (below the maximum allowable limit set by the Ministry of Food and Drug Safety, MFDS), whereas aflatoxin B2, G1 and G2 were not detected. Mycotoxins that are not regulated presently in Korea were also detected: fumonisin (0.84-14.25 ㎍/kg), ochratoxin A (0.76-17.42 ㎍/kg), and zearalenone (1.73-15.96 ㎍/kg). Risk assessment was evaluated by using estimated daily intake (EDI) and specific guideline values. These results indicate that the overall exposure level of Koreans to mycotoxins due to the intake of agricultural products used for food and medicine is unlikely to be a major risk factor for their health.