• Title/Summary/Keyword: Limit Of Quantitation

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A Fast Determination of Globotriaosylsphingosine in Plasma for Screening Fabry Disease Using UPLC-ESI-MS/MS

  • Yoon, Hye-Ran
    • Mass Spectrometry Letters
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    • v.6 no.4
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    • pp.116-119
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    • 2015
  • Globotriaosylsphingosine (lyso-Gb3) is considered as one of the biological marker for Fabry disease. To date, a reliable biomarker that reflects disease severity and progression has not been discovered to guide the management of Fabry disease. A new method included a simple protein precipitation with acetonitrile in 100 μL of plasma following analyte separation on an Phenomenex Kintex- C18 column using a gradient elution (0.1% formic acid in 5-90% acetonitrile). Total run time was within 12 min including sample preparation and MS/MS analysis. The limit of detection and limit of quantitation were 1 ng/mL and 2 ng/mL, respectively. The calibration curve was linear over the concentration range of 2.0-200.0 ng/mL (r2 = 0.9999). Inter-day accuracy and precision at 7 level were 93.4-100.7% with RSD of 0.55-5.97%. Absolute recovery was 97.6-98.6%. The method was applied to human and mice plasma, proved the suitability for quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.

Simultaneous Determination of Cysteamine and Cystamine in Cosmetics by Ion-Pairing Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Yejin;Na, Dong Hee
    • Toxicological Research
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    • v.35 no.2
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    • pp.161-165
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    • 2019
  • Cysteamine has been used in cosmetics as an antioxidant, a hair straightening agent, and a hair waving agent. However, recent studies indicate that cysteamine can act as an allergen to hairdressers. The objective of this study was to develop and validate a simple and effective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the measurement of cysteamine and its dimer, cystamine. Sodium 1-heptanesulfonate (NaHpSO) was used as an ion-pairing agent to improve chromatographic performance. Separation was performed on a Gemini C18 column ($250mm{\times}4.6mm$, $5{\mu}m$ particle size) using a mobile phase composed of 85:15 (v/v) 4 mM NaHpSO in 0.1% phosphoric acid:acetonitrile. UV absorbance was monitored at 215 nm. The RP-HPLC method developed in this study was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, and recovery. Cysteamine and cystamine were chromatographically resolved from other reducing agents such as thioglycolic acid and cysteine. Extraction using water and chloroform resulted in the recovery for cysteamine and cystamine ranging from 100.2-102.7% and 90.6-98.7%, respectively. This validated RP-HPLC method would be useful for quality control and monitoring of cysteamine and cystamine in cosmetics.

Automated On-Line Digestion System for the Determination of Total Phosphorus (총 인 분석을 위한 자동 전처리 시스템)

  • 정형근;조영일;김범식;박주형
    • Journal of Environmental Science International
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    • v.10 no.1
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    • pp.13-19
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    • 2001
  • An on-line digestion system based on the flow injection analysis technique was presented for the determination of total phosphorus. The system converts condensed and organic phosphoruses into orthophosphate that can be analyzed spectrophotometically. The reaction between orthophosphate and ammonium molybdate in a strong acid medium forms the yellow complex of phosphomolybdate which is next reduced to a molybdic blue complex by stannous chloride. The quantitation of orthophosphate is based on the absorbance of the molybdic blue. To determine total phosphorus, the digestion system was installed between the sample injector and the reaction coil with the added lines of digestion solution(potassium persulfate+sulfuric acid) and the $H_2O$ carrier. The system has shown that the digestion efficiencies were greater than 95% for the typical condensed and organic phosphoruses. When tripolyphosphate standards were used, the calibration data showed that the linear dynamic range extended to a concentration of 1.5ppm with the detection limit of 25ppb total phosphorus. The typical relative standard deviation was less than 2%. The proposed system was successfully applied to lake water, wastewater, and streamwater. The analytical variables such as digestion efficiency, analysis time, and reproducibility were evaluated and compared with the manual digestion method.

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Procedures in Establishing Residue Limits of Pesticides on Food Crops in Codex Alimentarius Commission and Foreign Countries (국제기구 및 외국에서 농산물중 농약잔류 허용기준의 설정절차)

  • Lee, Mi-Gyung;Hong, Moo-Gi;Park, Kun-Sang;Choi, Dong-Mi;Lim, Moo-Hyuk;Lee, Su-Rae
    • Korean Journal of Environmental Agriculture
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    • v.24 no.1
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    • pp.45-55
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    • 2005
  • This study was undertaken to find out necessary measures to improve the tolerance setting system of pesticide residues on food crops in Korea which is scientifically reasonable and harmonizable with international standards. Information on tolerance setting systems of pesticide residues by Codex Alimentarius Commission, Joint FAO/WHO Meeting of Experts on Pesticide Residues, USA, EU, Japan and Taiwan was collected and analyzed. On the basis of information in the above countries, necessary actions to be taken by the Korean regulatory authorities were recommended with respect to priority setting, maximum residue limits (MRLs) setting based on field residue data, group MRLs, minor crop problems, quantitation limit and dietary intake assessment.

Quantification of Allantoin in Yams (Dioscorea sp.) Using a 1H NMR Spectroscopic Method

  • Thao Quyen Cao;Dongyup Hahn
    • Journal of Microbiology and Biotechnology
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    • v.33 no.5
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    • pp.662-667
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    • 2023
  • Allantoin is an abundant component of yams and has been known as a skin protectant due to its pharmacological activities. In previous methods for allantoin determination using high-performance liquid chromatography (HPLC), the separation was unsatisfactory. We herein developed a 1H quantitative nuclear magnetic resonance (qNMR) method for quantification of allantoin in the flesh and peel of yams. The method was carried out based on the relative ratio of signals integration of allantoin to a certain amount of the internal standard dimethyl sulfone (DMSO2) and validated in terms of specificity, linearity (range 62.5-2000 ㎍/ml), sensitivity (limit of detection (LOD) and quantification (LOQ) 4.63 and 14.03 ㎍/ml, respectively), precision (RSD% 0.02-0.26), and recovery (86.35-92.11%). The method was then applied for the evaluation of allantoin in flesh and peel extracts of four different yams cultivated in Korea.

Quantitation and Validation of Atorvastatin using HPLC-UV

  • Heine, Daniel;Yong, Chul-Soon;Kim, Jung-Sun
    • Journal of Pharmaceutical Investigation
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    • v.37 no.3
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    • pp.187-192
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    • 2007
  • A reversed phase HPLC analysis of atorvastatin (AS) standard solution was performed using diclofenac (DF) as internal standard. Column oven temperature, flow rate and the composition of the mobile phase were varied in order to determine a practical system setup using a C18 column and UV detector. Two C18 columns of different length were compared regarding their influence on the AS peak shape. Based on these preliminary experiments a validation study was performed utilizing a C18 column at $62^{\circ}C$ with a mobile phase consisting of sodium phosphate buffer (0.05 M, pH 4.0), methanol and acetonitrile (40:50:10, v/v/v). The detection limit for AS was $0.1{\mu}g/ml$ and inter- and intra-day calibration curves were linear over a concentration range of $0.2-50{\mu}g/ml$. Accuracy and precision were satisfactory in the AS concentration range of $0.5-50{\mu}g/ml$.

HPLC Method Validation for Quantitative Analysis of Scopoletin from Hot-Water Extract Powder of Artemisia annua Linné (기능성 원료 인정을 위한 제출자료 작성 가이드[민원인 안내서]에 따른 개똥숙 열수추출분말의 Scopoletin 분석을 위한 HPLC 분석법 밸리데이션)

  • Kim, Seon-Hee;Yoon, Kee Dong
    • Korean Journal of Pharmacognosy
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    • v.51 no.1
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    • pp.78-85
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    • 2020
  • In this study, we shortly introduced the HPLC method validation guideline for the analysis of functional food which was released from the Ministry of Food and Drug Safety of Korea in Dec 2018. The HPLC method validation was performed through the aforementioned HPLC method validation guideline in order to quantitate scopoletin content from the hot-water extract powder of Artemisia annua Linné. The HPLC method was validated by evaluating specificity, accuracy, precision, limit of quantitation and linearity. All parameters were in the suitable ranges which are designated in the guideline, which indicated the current HPLC method is reliable to quantitate the scopoletin content from the hot-water extract of A. annua.

Pharmacokinetics of DA-8159, a new PDE5 inhibitor, after single and 1-week repeated oral administrations in mice

  • Park, Kyung-Jin;Ahn, Gook-Jun;Kim, Dong-Hwan;Shim, Hyun-Joo;Ahn, Byung-Ok;Kim, Soon-Hoe;Kim, Won-Bae
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.245.1-245.1
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    • 2003
  • DA-8159 is a new PDEV (Phosphodiesterase V) inhibitor, synthesized by Dong-A Pharm., as an oral agent to treat male erectile dysfunction. To make a selection of the dosage of oral administration in carcinogenic studies, we studied preliminarily the pharmacokinetics of DA-8159 after single (at the 1$\^$st/ day) and 1-week (at the 7$\^$th/ day) oral administrations of the drug at doses of 15, 50 and 150 mg/kg/day, to male ICR mice. In 15mg/kg single and 1-week repeated oral administration groups, the concentrations of DA-8159 and DA-8164(the main metabolite of DA-8159) were below the limit of quantitation(LOQ:50ng/ml). (omitted)

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A Simple Method for Determining Residual p-arsanilic Acid in Aquatic Products using EDTA-Assisted Solvent Extraction and LC-MRM

  • Min Kyeong Kwon;Ye Bin Shin;Young Min Kim;Jin Hwan Kim;Ji Seong Kim;Yong Seok Choi
    • Mass Spectrometry Letters
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    • v.14 no.2
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    • pp.36-41
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    • 2023
  • A simple method was developed to determine residual p-arsanilic acid (ASA), an organo-arsenic compound used as a feed additive, in aquatic products (eel, halibut, and shrimp) using EDTA-assisted solvent extraction and LC-MRM. The method was successfully validated in terms of specificity, linearity (coefficient of determination ≥ 0.995), accuracy (recovery or R, 72.72-78.73%), precision (the relative standard deviation of R, 2.08-6.98%), and sensitivity (the lower limit of quantitation, 5 ppb) according to CODEX guidelines (CAC-GL 71-2009). The use of EDTA in the extraction solvent and water with a suitable pH modifier as the reconstitution solvent may be the key factors for successful results. This is the first method that can be used for monitoring residual ASA in aquatic products using LC-MRM and could contribute to establishing a better aquatic product safety management system.

A Biotin-avidin Labeled Enzyme Immunoassay for the Quantitation of Serum TSH Using Protein-layered Solid Phase

  • Choi, Myung-Ja;Song, Eun-Young;Chung, Tai-Wha
    • Archives of Pharmacal Research
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    • v.21 no.3
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    • pp.231-235
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    • 1998
  • A sensitive enzyme immunoassay for serum TSH has been developed utilizing the tight binding between biotin and avidin, and three layered protein polystyrene beads as solid phase. To increase binding capacity of TSH and sensitivity of the assay, the polystyrene beads were coated sequentially with mouse immunoglobulin as first layer, rabbit antimouse immunoglobulin as second layer and monoclonal anti-TSH as third layer. A serum sample was incubated simultaneously with a monoclonal anti-TSH immobilized polystyrene beads and a second monoclonal anti-TSH covalently attached to biotin. After washing, the antibody bound serum TSH-anti-TSH-biotin complex is reacted with horseradish peroxidase (HRP)-labeled avidin. Following second wash, the bound HRP activity was measured calorimetrically. Reproducible results were obtained within 4 hours for serum TSH in the range between $0{\mu}\textrm{IU}$ml and ${50}{\mu}\textrm{IU}$ml with detection limit of $0.1{\mu}\textrm{IU}$ per test.

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