• 제목/요약/키워드: method detection limit

검색결과 1,360건 처리시간 0.033초

Validation and measurement uncertainty of HPLC method for simultaneous determination of 10 dyes in adulterated Phellodendron

  • Lim, Suji;Yun, Choong-In;Ko, Kyung Yuk;Kim, Young-Jun
    • 한국식품과학회지
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    • 제53권4호
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    • pp.391-398
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    • 2021
  • As global interest in herbal medicines has increased, the adulteration of herbal medicines has become a critical safety issue. Adulteration with dyes to improve the appearance of low-quality products is of particular concern. This study aimed to develop a high-performance liquid chromatography (HPLC) method to detect dyes added as adulterants to Phellodendron. Samples were analyzed on a C18 column using 50 mM ammonium acetate and acetonitrile as the mobile phase. All calibration curves showed good linearity (r2 ≥0.9999) over the five-point concentration range (1-50 mg/kg). Limit of detection ranged from 0.04-0.35 mg/kg, and limit of quantification ranged from 0.11-1.07 mg/kg. The repeatability and reproducibility for these measurements were 94.2-103.3% and 96.6-103.8% for accuracy and 0.14-2.28 RSD (%) and 0.80-2.37 RSD (%) for precision. Moreover, the measurement uncertainty of the low, medium, and high concentrations for 10 dyes was considered. Thus, this HPLC method is suitable for detecting color adulteration of Phellodendron.

러프집합과 퍼지 모델을 이용한 인공위성의 이상 동작 검출 시스템 (Satellite Anomalous Behavior Detection System through Rough-Set and Fuzzy Model)

  • 양승은
    • 한국위성정보통신학회논문지
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    • 제12권3호
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    • pp.35-40
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    • 2017
  • 위성의 상태를 파악하기 위해 기존에는 OOL(Out-Of-Limit) 방식을 많이 사용하여 왔다. OOL은 특정 텔레메트리의 상위, 하위 문턱 값을 지정하여 해당 값을 벗어날 경우 문제가 발생한 것으로 인식 하는 방식이다. 이 방법은 파라미터의 특성을 파악하여 각각의 문턱 값을 정확히 설정해야 하는 전문 지식과 노력이 필요하고 텔레메트리 값이 문턱값 내에서 비정상적으로 변할 경우는 검출할 수 없다는 문제점이 있다. 이러한 문제를 극복하기 위해 본 논문에서는 위성이 정상 상태일 때 텔레메트리의 통계적 특징 중 러프집합을 이용하여 중요한 것을 선택, 적용하여 퍼지 모델을 구축하고 이상 상태를 구분하는 시스템을 제안한다. 정상 상태의 데이터만 이용하여 모델을 구축하기 때문에 출력값을 비교 하여 사전에 정의되지 않은 비정상 상태의 구분이 가능 하며 다양한 통계 값을 이용하기 때문에 전문 지식 필요 없이 문턱값 내에서 비정상적으로 변하는 텔레메트리를 검출할 수 있다. 제안한 시스템의 동작 확인을 위해 실제 저궤도 관측위성의 배터리 온도 텔레메트리를 적용하여 시험을 수행 하였고 비정규적 운영 상태에 대한 검출이 성공적으로 이루어 졌다.

Simulation for Small Lamellar Grating FTIR Spectrometer for Passive Remote Sensing

  • Chung, You Kyoung;Jo, Choong-Man;Kim, Seong Kyu;Kim, In Cheol;Park, Do-Hyun;Bae, Hyo-Yook;Kang, Young Il
    • Journal of the Optical Society of Korea
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    • 제20권6호
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    • pp.669-677
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    • 2016
  • A miniaturized FTIR spectrometer based on lamellar grating interferometry is being developed for passive remote-sensing. Consisting of a pair of micro-mirror arrays, the lamellar grating can be fabricated using MEMS technology. This paper describes a method to compute the optical field in the interferometer to optimize the design parameters of the lamellar grating FTIR spectrometer. The lower limit of the micro-mirror width in the grating is related to the formation of a Talbot image in the near field and is estimated to be about $100{\mu}m$ for the spectrometer to be used for the wavelength range of $7-14{\mu}m$. In calculating the far field at the detection window, the conventional Fraunhofer equation is inadequate for detection distance of our application, misleading the upper limit of the micro-mirror width to avoid interference from higher order diffractions. Instead, the far field is described by the unperturbed plane-wave combined with the boundary diffraction wave. As a result, the interference from the higher order diffractions turns out to be negligible as the micro-mirror width increases. Therefore, the upper limit of the micro-mirror width does not need to be set. Under this scheme, the interferometer patterns and their FT spectra are successfully generated.

Duplex PCR을 이용한 토끼(Oryctolagus cuniculus)와 고양이(Felis catus) 육류의 동시 검출법 개발 (Development of Duplex PCR Method for Simultaneous Detection of Rabbit (Oryctolagus cuniculus) and Cat (Felis catus) Meats)

  • 홍연;김미주;양승민;유인숙;김해영
    • Journal of Applied Biological Chemistry
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    • 제58권4호
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    • pp.383-387
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    • 2015
  • 국내 유통 식품 수입 식품 중 토끼와 고양이 고기의 혼입 여부를 알아내고 불법 도축된 고양이 고기를 토끼 고기나 다른 고기로 속여 판매하는 것을 방지하기 위해 토끼와 고양이를 동시에 검출할 수 있는 polymerase chain reaction (PCR) 법을 개발하였다. 토끼와 고양이의 종 특이 프라이머는 미토콘드리아의 cytochrome b 유전자를 대상으로 하였고 개발된 프라이머를 가공식품에 활용하는 것을 고려하여 PCR 산물의 크기는 토끼 101 bp, 고양이 191 bp로 최소화 하였다. 프라이머의 특이성은 총 21종의 동물을 대상으로 검토하였다. 개발된 검출법의 검출 한계는 시료 DNA를 희석하여 PCR과 Bioanalyzer로 확인한 결과 토끼는 0.005 ng, 고양이는 0.0005 ng이었다.

아세틸아세톤 유도체화 시약과 HPLC를 이용한 미량 포름알데하이드 수질분석 (Determination of Trace Amounts of Formaldehyde in Water Using High Performance Liquid Chromatography and Acetylacetone as a Derivative Reagent)

  • 이기창;박재형;이원태
    • 대한환경공학회지
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    • 제37권2호
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    • pp.81-86
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    • 2015
  • 수중에 존재하는 포름알데하이드(formaldehyde)를 ${\mu}g/L$ 단위 농도까지 정량할 수 있는 간단한 분석법을 개발하였다. 시료 전처리시 유도체화 시약으로 아세틸아세톤(acetylacetone)을 사용하였고, 기존 분석방법과 달리 추출 및 농축과정을 거치지 않는 것이 장점이다. 시료에 유도체화 시약을 첨가하고 $80^{\circ}C$에서 30분 반응시킨 후 HPLC를 이용하여 포름알데하이드를 분석하였다. 본 방법에 대한 정도보증 결과, 방법검출한계 및 정량한계는 각각 1.6, $5.0{\mu}g/L$로 기존 분석법에 비하여 낮았다. 정밀도 및 정확도는 각각 0.6~3.0%, 91.6~106.3%로 우수하였다. 또한 다양한 환경시료에 대한 회수율 검증에서도 92.0~115.2%로 양호하게 나타났다.

노로바이러스 검출을 위한 측면유동면역분석법 기반의 바이오리셉터 선별기법 개발 (Norovirus Targeted Bioreceptor Screening Method based on Lateral Flow Immunoassay (LFIA))

  • 장희수;조현지;전태준;김선민
    • 한국가시화정보학회지
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    • 제20권3호
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    • pp.136-145
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    • 2022
  • Later flow immunoassay (LFIA) is a protein analytical method based on immunoreaction. On the LFIA based protein analytical method, bioreceptor molecule plays a key role, and so a system that evaluates and manages the binding affinity of bioreceptor is needed to secure detection reliability. In this study, Lateral Flow Immunoassay based rapid Bioreceptor Screening Method (rBSM) is presented that provide a simple and quick evaluating method for the binding affinity to the target protein of the antibody as model bioreceptor. To verify this evaluation method, Virus-like particles (VLP) and anti-VLP antibodies are selected as a model norovirus, which is target protein, and the candidate bioreceptors respectively. Among the 5 different candidate antibodies, appropriate antibody could be sorted out within 30 minutes through rBSM. In addition, selected antibodies were applied to two representative LFIA based techniques, sandwich assay and competitive assay. Among these methods, sandwich assay showed more effective VLP detection method. Through applying selected antibodies and techniques to the commercialized mass production lines, an VLP detecting LFIA kit was developed with a detection limit of 1012 copies/g of VLPs in real samples. Since this proposed method in this study could be easily transformable into other combinations with bioreceptors, it is expected that this technique would be applied to LFIA kit development system and bioreceptor quality management.

MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석 (Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs)

  • 서계원;이재일;이채용;이정치
    • 한국식품위생안전성학회지
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    • 제18권2호
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

Chiral Purity Test of Bevantolol by Capillaryelectrophoresis and High Performance Liquid Chromatography

  • Long, Pham Hai;Trung, Tran Quoc;Oh, Joung-Won;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • 제29권9호
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    • pp.808-813
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    • 2006
  • Two methods for the chiral purity determination of bevantolol were developed, namely capillary electrophoresis (CE) using carboxymethyl-${\beta}$-cyclodextrin (CM-${\beta}$-CD) as a chiral selector and high-perfomance liquid chromatography (HPLC) using a chiral stationary phase. In the HPLC method, the separation of bevantolol enantiomers was performed on a Chiralpak AD-H column by isocratic elution with n-hexane-ethanol-diethylamine (10:90:0.1, v/v/v) as mobile phase. In the CE method, bevantolol enantiomers were separated on an uncoated fused silica capillary with 50 mM amonium phosphate dibasic adjusted to a pH 6.5 with phosphoric acid containing 15 mM CM-${\beta}$-CD as running buffer. Validation data such as linearity, recovery, detection limit, and precision of the two methods are presented. The detection limits of S-(-)-bevantolol were 0.1% and 0.05% for CE and HPLC method, respectively and R-(+)-bevantolol were 0.15% and 0.05% for CE and HPLC method, respectively. There was generally good agreement between the HPLC and CE results.

흑삼에서 벤조피렌의 추출 조건 및 분석 방법에 관한 연구 (Study on Extraction Condition and Analysis Methods of Benzopyrene in Black Ginseng)

  • 조영호;송규용;백명기;이종화;이계원
    • 약학회지
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    • 제56권3호
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    • pp.145-151
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    • 2012
  • To develop fundamental data of herbal materials with heat treatment, we studied analytical and extraction methods of benzopyrene in black ginseng and validated by HPLC analysis. Benzopyrene was successfully separated in mobile phase of acetonitrile:water (80 : 20) and detection of excitation 294 nm, emission 404 nm. The calibration curve of benzopyrene was linear over the concentration range of 1.17~37.50 ng/ml with correlation coefficient of above 0.999. The limit of detection (LOD) and quantitation (LOQ) of benzopyrene was 0.25 and 0.75 ng/ml, respectively. Hexane extraction method was used as a new extraction method for benzopyren and the efficient of extraction was over 95%. In conclusion, analytical method and extraction method were suitable for the determination of benzopyrene in the black ginseng and could be applied to fundamental study and guideline of herbal materials with heat treatment.

인체 혈장에서 염산시프로플록사신(시프로플록사신으로서 250 mg) 정량을 위한 HPLC 분석법의 유효성검토 (Validation of a Simple HPLC Method for Determination of Ciprofloxacin Hydrochloride in Human Plasma)

  • 하용화;조성희;천성국;서성훈;류재환;최영욱;이경태
    • Journal of Pharmaceutical Investigation
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    • 제34권4호
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    • pp.327-331
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    • 2004
  • A simple HPLC method with ultraviolet detection of ciprofloxacin in human plasma was developed and validated. After protein precipitation with trichloroacetic acid, chromatographic separation of ciprofloxacin in plasma was achieved at $50^{\circ}C$ with a $C_{18}$ column and methanol-phosphate mixture (pH 2.5), as mobile phase. Quantitative determination was performed by ultraviolet detection at 278 nm. The method was specific and validated with a limit of quantification of 100 ng/ml. The intra- and inter-day coefficients of variation were between 1.67% and 10.55% and accuracy between 92.01 % and 106.09%. The method has been successfully applied in a bioavailability study of 250 mg ciprofloxacin hydrochloride tablet.