• Title/Summary/Keyword: 분석검출한계

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Analysis of Biurea Decomposed from Azodicarbonamide in Food Products by High Performance Liquid Chromatography Mass/Mass Spectrometry (LC/MS/MS를 이용한 식품 중 아조디카르본아미드 분해산물인 Biurea 함량 분석)

  • Lim, Ho-Soo;Pahn, Kyeong-Nyeo;Kim, Jun-Hyun;Jang, Gui-Hyeon;Moon, Gui-Im;Yang, Hyo-Jin;Park, Sung-Kwan;Park, Hae-Kyong;Kim, So-Hee
    • Korean Journal of Food Science and Technology
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    • v.42 no.4
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    • pp.377-382
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    • 2010
  • This study was conducted to establish a method to analyze biurea decomposed from azodicarbonamide in processed foods such as wheat flour and bread. New method was developed using high performance liquid chromatography mass/mass spectrometry to determine biurea in wheat flour and bakery products. The recovery rate was 94.3-112.5%. The limit of detection for biurea was 0.003 mg/kg, and the limit of quantification was 0.01 mg/kg. The monitoring results for biurea content using established methods showed that biurea was detected at 2.76 mg/kg in the azodicarbonamide-detected flour (detection rate, 2%). The detection rate in processed foods such as baked goods was 27% (16/59). The detection range was 0.19-18.01 mg/kg (average, 3.79 mg/kg). However, it was thought that the detection level was safe due to much lower values than the standard (45 mg/kg). As a result, the newly established biurea analytical method will contribute to the management of azodicarbonamide in processed foods such as wheat flour and bakery products.

Monitoring of Preservatives Produced Naturally in Vegetable Raw Materials (식물성 원료 중 천연유래 보존료의 함유량 조사)

  • Soo Bin Lee;Ji Sun So;Geum Jae Jeong;Hye Seon Nam;Jae Myeong Oh;Soon Ho Lee
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.152-162
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    • 2024
  • In this study, we investigated the levels of the natural preservatives, benzoic acid, sorbic acid, and propionic acid, in raw unprocessed vegetables. Quantitative analysis of benzoic acid and sorbic acid was performed using high-performance liquid chromatography with a diode array detector (HPLC-DAD) and confirmed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and confirmed using gas chromatography-mass spectrometry (GC-MS). From a total of 497 samples, benzoic acid, sorbic acid, and propionic acid were found in 50 (10%), 8 (0.2%), and 61 samples (12.3%), respectively. The highest quantity of benzoic acid, sorbic acid, and propionic acid was found in peony root (1,057 mg/kg), nut-bearing torreya seeds (27.3 mg/kg), and myrrha (175 mg/kg), respectively. The background concentration range of naturally occurring preservatives in raw vegetables determined in this study could be used as standard inspection criteria to address consumer complaints and trade disputes.

Modification and Validation of an Analytical Method for Dieckol in Ecklonia Stolonifera Extract (곰피추출물의 지표성분 Dieckol의 분석법 개선 및 검증)

  • Han, Xionggao;Choi, Sun-Il;Men, Xiao;Lee, Se-jeong;Oh, Geon;Jin, Heegu;Oh, Hyun-Ji;Kim, Eunjin;Kim, Jongwook;Lee, Boo-Yong;Lee, Ok-Hwan
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.143-148
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    • 2022
  • This study was to investigate an analytical method for determining dieckol content in Ecklonia stolonifera extract. According to the guidelines of International Conference on Harmonization. Method validation was performed by measuring the specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) of dieckol using high-performance liquid chromatography-photodiode array. The results showed that the correlation coefficient of calibration curve (R2) for dieckol was 0.9997. The LOD and LOQ for dieckol were 0.18 and 0.56 ㎍/mL, respectively. The intra- and inter-day precision values of dieckol were approximately 1.58-4.39% and 1.37-4.64%, respectively. Moreover, intra- and inter-day accuracies of dieckol were approximately 96.91-102.33% and 98.41-105.71%, respectively. Thus, we successfully validated the analytical method for estimating dieckol content in E. stolonifera extract.

Simultaneous Determination of Organo-phosphorus and Organo-chlorinated Pesticides in Soil and Lawn Samples of Golf Courses (골프장 토양 및 잔디 시료 중 유기인 및 유기염소계 농약의 동시 분석)

  • Seo, Yong-Chan
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.12
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    • pp.1257-1262
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    • 2005
  • Organo-chlorinated pesticides have been seldom measured in Korea because their use was banned for more than two decades. Nevertheless, the environmental persistency of these pesticides requires regular monitoring. Only organo-phosphorus pesticides are currently being monitored in Korea. Simultaneous determination of organo-chlorinated and organo-phosphorus pesticides was attempted using gas chromatography/mass spectrometer detector. Pressurized fluid extraction(PFE) was used in sample preparation. PFE showed equivalent extraction efficiency to traditional soxhlet extraction with less solvent use and less sample preparation time. Average recovery of spiked pesticides to soil and lawn samples was 62% ranging 52 to 154%. Method detection levels(MDLs) for these pesticides ranged from 3.4 to 10.5 ${\mu}g/kg$. Endosulfan, fenitrothion, and diazinon were found in the samples from 5 different golf courses out of 9 courses.

HPLC를 이용한 축육(Pork Muscle)내의 Dihydrostreptomycin 검출법

  • Choe, Ji-Hyeon;Han, Eun-Yeong;Park, Jin-Gwan;Lee, Su-Yeon;Choe, Dong-Mi;Sin, Ho-Cheol;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.196-203
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    • 2005
  • 축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

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Detection of Hepatitis B Virus by LAMP and DHPLC (등온증폭반응법과 변성 고성능 액체 크로마토그래피를 이용한 B형 간염 바이러스의 검출)

  • Ahn, Young-Chang;Seo, Jae-Won;Choi, Jae-Gu;Jang, Won-Cheoul
    • Journal of the Korean Chemical Society
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    • v.55 no.2
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    • pp.262-267
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    • 2011
  • The denaturing high performance liquid chromatography(DHPLC) with fluorescence detector assay is very useful tool for detecting nucleic acids. Furthermore, loop-mediated isothermal amplification(LAMP) constitutes a potentially valuable tool for rapid diagnosis of pathogenic microorganisms. In this study, we evaluated the specificity, detection limit, and sensitivity of a LAMP method and DHPLC method for rapid detection of the hepatitis b virus(HBV). As a result, the LAMP assay reported here has the advantage of rapid detection whereas, DHPLC assay has more sensitivity than other assays. These findings suggest that LAMP and DHPLC assay may be good tool for rapid diagnosis of clinical HBV infection.

Shot Boundary Detection Model using Knowledge Distillation (지식의 증류기법을 이용한 샷 경계 검출 모델)

  • Park, Sung Min;Yoon, Ui Nyoung;Jo, Geun-Sik
    • Proceedings of the Korean Society of Broadcast Engineers Conference
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    • 2019.06a
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    • pp.29-31
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    • 2019
  • 샷 경계 검출(Shot Boundary Detection)은 영상 콘텐츠 분석을 위한 필수적인 기술이며, 다양한 방식으로 편집된 영상의 샷 경계를 정확하게 검출하기 위한 연구가 지속되어 왔다. 그러나 기존에 연구들은 고정된 샷 경계 검출 알고리즘이나 매뉴얼한 작업과 같이 학습이 불가능한 과정이 포함되어 있어 성능 개선에 한계가 있었다. 본 논문에서는 이러한 과정을 제거한 End-to-End 모델을 제안한다. 제안하는 모델은 시공간 정보 추출성능을 높이기 위해 행동 인식 데이터셋을 이용한 전이학습을 사용하고, 샷 경계 검출 성능을 높이기 위해 개선된 지식의 증류기법(Knowledge Distillation)을 결합한다. 제안하는 모델은 ClipShots 데이터셋에서 DeepSBD 에 비해 cut transition 과 gradual transition 이 각각 5.4%, 41.29% 높은 성능을 보였고, DSM 과의 비교에서 cut transition 의 정확도가 1.3% 더 높은 결과를 보였다.

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HPLC를 이용한 우유 중에 잔류 항생물질(Streptomycin)의 정량 분석

  • Byeon, Jang-Won;Park, Hwan-Seok;Hong, Go-Eun;Hong, Mu-Gi;Park, Gwan-Ha;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.310-316
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    • 2005
  • 축산식품(우유)내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/dihydrostreptomycin, neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 STP에 대한 HPLC법에 대한 보고한 Edder 방법 중에 clean-up 과정 및 이동상 조건을 대폭 수정하여 STP의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering La-boratories, Inc.)의 컬럼 온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, 유도체화 용매 유속 0.6ml/min 이동상 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 STP 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 STP의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection(LOD)은 0.02ppm이었으며, 적어도 우유에서의 MRL이 0.6ppm임을 감안하면 STP를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 우유에 표준 STP를 0.5ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.

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Analysis of Butyltin Compounds(mono-, di-, and tributyltin) in Human Blood (혈액 중의 주석화합물(MBT, DBT, TBT)의 분석과 농도에 관한 연구)

  • Kim, Nam Sook;Park, Dong Uk;Oh, Jae Ryoung;Shim, Woon Joon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.115-122
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    • 2001
  • Butyltin compounds, including mono-(MBT), di-(DBT) and tributyltin(TBT) were analyzed in 44 human blood samples randomly collected from a hospital in "K" a city. Gas chromatograph equipped with flame photometric detector(FPD) was used to quantify the amounts of butylin compounds. Method detection limits(MDL) of this analytical method were 3.69ng Sn/g for MBT, 0.91ng Sn/g for DBT and 1.09ng Sn/g wet wt for TBT respectively. Standard reference material(SRM) containing of $1.3{\mu}g/g$ TBT as chloride was analyzed to check if this analytical results would be reliable. Recovery of about 90% was obtained through this analysis, indicating that the analytical method from butyltin compounds blood was reliable. The concentrations of butyltin compounds ranged MDL(<3.69) to 7.93ng Sn/g for MBT and 1.15 to 5.41ng Sn/g wet wt for DBT. Tributyltin was below detection limit in all samples. Detection limits of our results are lower than those reported by Kannan et al. who reported butyltin compounds in 33 human blood samples in the United States. Detection of MBT and DBT on blood sample implies that butyltin compounds could be absorbed through consumption of seafoods or exposure to food stuffs made of plastics and household items. Further study is needed to examine if butyltin compounds in blood can be reliably analyzed and used as intake index.

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A Study on the Determination of Rare Earth Elements by Inductively Coupled Plasma Spectrometry (Inductively Coupled Plasma 법을 이용한 희토류원소의 분석에 관한 연구)

  • Beom Suk Choi;Sun Tae Kim;Young Man Kim;Chong Wook Lee
    • Journal of the Korean Chemical Society
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    • v.29 no.4
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    • pp.382-389
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    • 1985
  • The effect of plasma operational parameters for the determination of rare earth elements(REE) by means of inductively coupled plasma(ICP) spectrometry was investigated. While the increase in the flow rate of carrier gas argon enhanced the sensitivity and lowered the detection limit, significant ionization interferences were observed. The decrease in RF power increased the signal to background ratio. The observation point showing the lowest ionization interference was slightly higher than the position where the spatial profile of the analyte reached the maximum. The detection limits of the spectral lines commonly used for the determination of REE were measured and the spectral lines relatively free from spectral interferences were chosen.

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