• 제목/요약/키워드: 정량검출한계

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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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수돗물 바이러스 논쟁 : 바이러스의 실재와 위험 인식의 구성

  • Seong, Ha-Yeong
    • Journal of Science and Technology Studies
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    • v.7 no.2
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    • pp.125-154
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    • 2007
  • 1997년부터 2002년까지 수돗물의 바이러스 오염 여부에 관한 논쟁이 있었다. 서울대의 K 교수는 학회에서 수돗물을 분석한 결과 질병을 일으키는 바이러스가 검출되었다고 보고했고, 이 내용이 언론을 통해 보도되면서 수돗물의 안정성에 대한 논쟁이 일어났다. 이 논쟁은 바이러스 검출방법론의 신뢰성을 둘러싼 과학적 논쟁과 검출된 바이러스가 위험한지에 대한 위험논쟁이 함께 공존하며 진행되었다. 필자는 정책의 변화를 요구하는 과학적 사실을 둘러싼 논쟁을 분석하기 위해 과학전문가와 정부를 분석의 대상으로 삼고 있으며, 아래의 세 가지를 주장하고 있다. 첫째, 논쟁을 제기한 과학자(K 교수)와 정부(환경부, 서울시)가 바이러스의 확인부터, 승인, 정책 결정에 이르는 전 과정에서 검출방법론에 차이를 보이고 있으며, 이러한 방법의 차이는 민감성과 정확성을 추구하는 과학계와 법적기준을 위한 정량적 가치를 중시하는 정부의 특징이 반영된 것임을 주장한다. 둘째, 과학논쟁에서 K 교수팀이 PCR 방법을 통해 바이러스의 실재(reality)를 확인하면서 과학적 정당성을 확보했음을 보인다. 셋째 바이러스의 검출 방법에서 PCR 방법이 과학적 실재를 결정했지만, 위험의 실재를 규정하는 데에는 한계가 있었음을 지적한다. 마지막으로 본 논문은 논쟁분석을 통해 정책입안을 둘러싼 과학 위험논쟁에서 과학전문가의 역할을 고찰하고 있다.

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Gas-Sensing Membrane Electrodes for the Determination of Dissolved Gases (I). Continuous-Automated Determination of Nitrite Ion Using Tubular PVC Membrane Type of pH Electrode (용해기체 분석용 기체 감응막 이온선택성 전극 (제 1 보). 관형 PVC 막 pH 전극을 이용한 아질산이온의 연속·자동화 정량)

  • Heung Lark Lee;Jong Hoon Yun
    • Journal of the Korean Chemical Society
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    • v.33 no.4
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    • pp.388-398
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    • 1989
  • A continuous-automated method for the determination of nitrite ion using gas-sensing membrane electrode was developed. The pH electrode of tubular PVC membrane type was used as a detector of this system. The slope of linear response of the electrode measured at optimum conditions for the continuous-automated determination of nitrite ion was 63.5 mV/decade. The concentration range of linear response and detection limit were 2.5 ${\times}10^{-4}{\sim}\;7.5{\times}10^{-2}$M and $8.0{\times}10^{-5}$M, respectively. This detection system was not only less interfering to acidic gas species than other methods but also less time consumable for determination.

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Analytical Method Development for Determination of Coenzyme Q10 by LC-MS/MS in Related Health Functional Foods (건강기능식품에서 LC-MS/MS를 이용한 코엔자임Q10 분석법 연구)

  • Lee, Jin Hee;Oh, Mihyune
    • Journal of Food Hygiene and Safety
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    • v.34 no.6
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    • pp.519-525
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    • 2019
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we are continuing our research on analytical method development for the items listed in the Korean Health Functional Food Codex. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determine coenzyme Q10 based on liquid chromatographic-tandem mass spectrometry (LC-MS/MS). Calibration curves showed linearity with a correlation coefficient (R2) of > 0.999 and the limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 26.0 ㎍/L and 78.9 ㎍/L, respectively. The recovery results ranged between 98.6-107.0% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high resolution of the coenzyme Q10 and the assay was fully validated as well.

Simultaneous Analysis of Multi-Residual Pesticides Using UPLC (UPLC를 이용한 잔류농약 다성분 동시분석 연구)

  • Kim, Ki-Yu;Eom, Mi-Na;Kang, Jung-Bok;Do, Young-Suk;Moon, Su-Gyeong;Jung, Il-Hyeong;Son, Jong-Sung;Pi, Il-Seon;Park, Eun-Mi;Kim, Young-Su;Lee, Seong-Bong;Cho, Sang-Hun;Moon, Sun-Ae
    • Bulletin of Food Technology
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    • v.21 no.2
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    • pp.49-54
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    • 2008
  • 농산물 중 잔류농약을 보다 쉽고 효율적으로 분석 할 수 있는 다성분 동시분석 방법에 따라서 UPLC-PDA을 이용하여 기기조건에 따른 검출한계 및 정량한계를 식품별 최저 MRL과 비교하여 유효성을 알아보고 회수율을 통하여 방법의 재현성을 조사한 결과 다음과 같다. 41종의 농약에 대한 검량선은 직선성이 우수하였으며 검출한계 $0.005{\sim}0.109mg/kg$으로 나타났으며 정량한계 는 $0.018{\sim}0.363ppm$으로 나타났다. Cycloprothrin 등의 경우처럼 검출기의 감응도가 최저 MRL 기준을 초과하는 농약에 대한 보완으로는 검출감도가보다 우수한 UV 검출기 등의 병행 활용이 필요하다. 회수율에 따른 재현성은 쌀의 경우 첨가 농도 0.4 mg/kg 일때 $62.09{\sim}99.58%$로 편차범위는 $1.03{\sim}13.92%$ 얻을 수 있었다.

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Determination of fucoxanthin in cosmeceutical products by HPLC-PDA (HPLC-PDA를 이용한 기능성 화장품 중 푸코잔틴의 정량)

  • Choi, Jongkeun
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.18 no.12
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    • pp.755-761
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    • 2017
  • This study was conducted to establish an analytical method using an HPLC system equipped with a photodiode array (PDA) detector for the quality control of raw materials and cosmeceuticals containing fucoxanthin as an active ingredient. The column was octadecyl-functionalized silica gel and the measurement wavelength of the PDA was set to 499 nm. To validate the analytical method, the linearity of the calibration curve, detection limit, reproducibility and recovery rate were investigated and good results were obtained. The correlation coefficient of the calibration curve was 1.000 and the linearity was good in the concentration range of 0.5 ~ 100 ppm. Moreover, the limit of detection (LOD) was 0.1 ppm and the limit of quantification (LOQ) was 0.5 ppm. The results of the peak reproducibility test used for evaluating the system suitability showed that the RSD (n = 5) of the peak area was 2.0% and that of the retention time was 0.09%. In the spiking test, the recovery rate was $101.6{\pm}0.77%$. The fucoxanthin contents of the two kinds of fucoxanthin-containing raw materials were $49.6{\pm}3.3%$ and $1.03{\pm}0.016%$, respectively. In addition, the fucoxanthin content in the test product, which was intended to be 150 ppm, was $156.7{\pm}4.7ppm$. From the above results, it was concluded that this method could be applied to the quantitative analysis of fucoxanthin in cosmeceuticals.

Determination of Histidine by Spectrofluorometry (형광광도법에 의한 Histidine의 정량에 관한 연구)

  • Cha, Ki Won;Huang, Huazi
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.180-183
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    • 2004
  • A simple and sensitive determination method of histidine has been investigated using the spectrofluorometry. An emission peak of $Eu^{3+}$ - TTA- histidine complex occurs at 470 nm in aquous solution with excitation at 235 nm and the fluorescence intensity increased linearly with addition of histidine in the range of $1{\times}10^{-7}-4{\times}10^{-6}M$. The detection limits was $5{\times}10^{-7}M$ with 3.5% RSD. The present method was applied to determine histidine content in the synthetic sample.

Real-time PCR assay for the Detection of Toxoplasma gondii in Retail Meats: Proof-of-concept Study (유통식육에서의 톡소포자충 검출을 위한 유전자검사법 개발)

  • Yun, Han Seong;Suh, Soo Hwan;Kwak, Hyo-Sun;Joo, In-Sun
    • Journal of Food Hygiene and Safety
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    • v.32 no.3
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    • pp.199-205
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    • 2017
  • Although many PCR-based assays have been developed, the majority of rapid detection of Toxoplasma gondii in animal and their meat product has been dependent on immunogenic assays. Thus, there is still a need for more reliable PCR based detection method for T. gondii in retail meats. Recently, a 529-bp repeat element that exists in 200-300 copies per genome of T. gondii genome had been spotlighted for its usefulness as potential detection targers. In this study, the 529-bp repeat element was selected for real-time PCR to detect three types of T. gondii (type I, II and III). A primer pair targeting 82-bp of the 529-bp element detected all three types of T. gondii and showed high level of specificity against 14 different food-borne pathogens as well as 3 protozoan parasites such as Giardia lamblia, Cryptosporidium parvum and Entamoeba histolytica. Application of the new real-time PCR assay in meat samples showed improved detection sensitivity compared to the B1-gene targeted method suggesting potential new target for Toxoplasma gondii screening in retail meats.

Development of Ceramide NP Analysis Method in Cosmetic Formulations Using Liquid Chromatography (액체크로마토그래피를 이용한 화장품 제형 내 세라마이드엔피 분석법 확립)

  • Ye Ji Lee;Young Eun Kim;Jae Yong Seo;Hyun Dae Cho
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.49 no.4
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    • pp.291-298
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    • 2023
  • In this study, a quantitative analysis method was developed using high-performance liquid chromatography (HPLC) to analyze the content of ceramide NP in lotion, cream, and cleanser formulations in cosmetics. The analysis was performed using a C18 column, and the mobile phase was set at a ratio of 70 : 30 for acetonitrile and methanol, the flow rate was set to 0.8 mL/min, and the column temperature was set to 20 ℃. The method was verified by analyzing specificity, linearity, limit of detection, limit of quantitation, accuracy, and precision in accordance with the ICH guidelines. As a result of validating the method, the linearity of the calibration curve was excellent (R2 = 0.99984). The accuracy of the lotion, cream, and cleanser formulations was confirmed with a recovery rate ranging from 95.11% to 100.48%. The precision analysis showed a low relative standard deviation (RSD) of less than 0.26%. The limit of detection was 0.902 ㎍/mL, and the limit of quantitation was 2.733 ㎍/mL. Through this quantitative analysis method of ceramide NP applied in cosmetics, it is expected to assist in the quality control of products by enabling measurement even when it is difficult to separate the main peak due to the influence of interfering substances.

Determination of Oxolinic Acid Residues in Acetes japonicus by HPLC (보리새우에 잔류하는 Oxolinic Acid HPLC를 이용한 검출법)

  • 이문한;임재영;정순관;손성완;박종명
    • Journal of Food Hygiene and Safety
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    • v.8 no.3
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    • pp.147-150
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    • 1993
  • A novel rapid and sensitive method to detennine residual oxolinic acid in Acetes japonicus was developed. The residual oxolinic acid was extracted with ethylacetate and diluted oxalic acid, and interfering substances were removed by hexane. Fifty ppb residual concentration in the extract could be quantitated by UV-HPLC and the recovery rates were 79-91% according to the fortified amounts.

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