• Title/Summary/Keyword: Method detection limits

Search Result 596, Processing Time 0.032 seconds

Simultaneous Determination of Avicularin and Quercitrin in Astilbe chinensis by HPLC

  • Seo, Changon;Jung, Yeon Woo;Kwon, Jin Gwan;Hong, Seong Su;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Choi, Chun Whan;Kim, Jin Kyu
    • Proceedings of the Plant Resources Society of Korea Conference
    • /
    • 2019.04a
    • /
    • pp.102-102
    • /
    • 2019
  • This study developed a HPLC analysis method for the determination of avicularin (AL) and quercitrin (QT) in Astilbe chinensis by HPLC. HPLC was performed on a Capcell Pak C18 MGII column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$ and a UV detection wavelength of 254 nm. The analytical method was validated for its specificity, precision, accuracy, and linearity. The limits of detection and quantitation were AL 0.09 and 0.28 mg/mL, QT 0.03 and 0.09 mg/mL respectively. Calibration curves showed good linearity (AL r2 > 0.99990 and QT r2 > 0.99994), and the precision of analysis was satisfied (less than AL 0.59%, QT 0.63%). Recoveries of quantified compounds ranged from AL 100.57 to 102.08%, QT 99.94 to 100.64%. These results indicate that the developed HPLC method was applied successfully to the detection of AL and QT in A. chinensis.

  • PDF

Identification of Standard Compound of Ja-ha-guh Pharmacopuncture and Validation of Analytic Methods (자하거 약침의 지표물질 선정 및 분석법 벨리데이션)

  • Park, Sang-won;Lee, Jae-woong;Lee, Jin-ho;Ha, In-Hyuk;Byun, Jang-hoon;Jung, Bum-hwan;Jung, Hwa-jin;Lee, In-hee;Kim, Min-Jeong;Kim, Eun-Jee
    • Journal of Korean Medicine Rehabilitation
    • /
    • v.26 no.1
    • /
    • pp.33-40
    • /
    • 2016
  • Objectives Despite the increasing use of Ja-ha-guh (Hominis-placenta ) pharmacopuncture in rehabilitative medicine field, its standard compound has yet to be investigated. The purpose of this study is to provide standardization for future studies and increase satisfaction of patients by utilizing standard pharmacopuncture. Methods Alanine and leucine were selected as potential standard compounds. LC/MS was used to devise an analytic method. This analytic method was subject to validation. According to validation guideline of Korea Food and Drug Administration, the specificity, linearity, precision, range, quantitative limits, detection limits and accuracy were measured. With this analysis, 3 lots of Ja-ha-guh pharmacopuncture were analyzed. Results Because the specificity, linearity, precision, range, quantitative limits, detection limits and accuracy meet criteria of the guideline, the analytic method was validated. It was found that Ja-ha-guh pharmacopuncture contained $211.02{\pm}7.28ug/ml$ of alanine and $372.03{\pm}7.58ug/ml$ of leucine. Conclusions Both alanine and leucine appear to be suitable standard compounds. These results are likely to contribute to further standardization of Ja-ha-guh for medical use.

A Comparative Study of the Detectable Methods of Residual Antibiotics in Milk (우유중 잔류 항생물질 분서방법에 관한 비교연구)

  • 백선영;김형일;박건상;김소희;권경란
    • Journal of Food Hygiene and Safety
    • /
    • v.11 no.2
    • /
    • pp.129-132
    • /
    • 1996
  • Recently, as concern about the residual antibiotics in milk increase, the detection methods of residual antibiotics used extensevely at the present time were investigated and compared to their properties and the detection limits of variable antibiotics. At first, comparactive tests of the detectable sensitivity of 4 test organisms, B. cereus, B. subtilis, M.luteus, B.stearothermophilus C-953, were performed by disc assay. As a result, B.stearothermophilus was the most sensitive strain of all other strains and showe the detect limit of 5-50 ppb for penlicillins (PCs). And also, B.subitilis was showed the more effective detection limit, 200-400 ppb, for aminoglycosides (AGs) and M.luteus was showed predominant sensitivity , 50-500 ppb for macrolides(MLs) and B.cereus was the most sensitive strain for tetracyclines (TCs) and showed the detection limit of 100-400 ppb. Therefore, each test strains were showed a different sensitivity in the detection of the different antibiotic families. When the detection limit of disc assay and other methods were compared, TTCmethod was less sensitive than other methods showing 5-50 ppb detectable lebel for PCs. Also, for the detection of other antibiotic families TTC method was showed the worst sensitivity and Delvo and Charm Farm tests were similar to the detectable properties of AGs and MLs. Although disc assay was showed the similar detection limit for PCs with Delvo and Charm Farm, it was more widely effective for the detection of kanamycin, erythromycin, chlortetracycline, doxycycline, verginiamycin and so on than Delvo or Charm Farm. CharmII test was showed the best sensitivity for the most of antibiotics except neomycin and gentamycin. But it was necessary that different tests must be performed to each antibiotic family and so it was regarded that the effectiveness of that method was low.

  • PDF

Ex Vivo Assay of Trace Nicotine Using a Voltammetric Modified Biosensor

  • Ly, Suw Young;Jang, Myung-Ho;Cha, Jae-Min;Kim, Min-Young;Oh, Hyun-Seok;Jo, Dong-Hyeon;Choi, Seong-Sik
    • Journal of the Korean Applied Science and Technology
    • /
    • v.29 no.1
    • /
    • pp.40-46
    • /
    • 2012
  • In vivo nicotine is associated with Alzheimer's, Parkinson's and lung cancer. Diagnostic assays of these diseases depend on very low analytical detection limits. In this study, a sensitive analytical method was examined using a voltammetric graphite pencil electrode (GPE) and a modified carbon nanotube paste electrode (CNE). The optimum analytical conditions for both electrodes were compared using square wave anodic stripping voltammetry (SW) and cyclic voltammetry (CV) obtaining 400 sec accumulation time and oxidation peak. Under optimum parameters, the stripping working range of GPE was $5.0-40.0{\mu}g/L$, CNE: 0.1-0.8 and $5-50{\mu}g/L$. Quantification limits were $5.0{\mu}g/L$ for GPE and $0.1{\mu}g/L$ for CNE, while detection limits were $0.6{\mu}g/L$ for GPE and $0.07{\mu}g/L$ for CNE. A standard deviation of $10.0{\mu}g/L$ was observed for 0.064 GPE and 0.095 CNE (n = 12) using 400 sec accumulation time. The results obtained can be applied to non.treated urine and ex vivo biological diagnostics.

Simultaneous Determination of Sulfonamides in Porcine and Chicken Muscle Using High Performance Liquid Chromatography with Ultraviolet Detector

  • Shim, You-Sin;Shin, Dong-Bin;Cho, Yong-Sun;Choi, Yun-Hee;Lee, Sang-Hee
    • Food Science and Biotechnology
    • /
    • v.18 no.6
    • /
    • pp.1430-1434
    • /
    • 2009
  • The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of $50-150\;{\mu}g/kg$ was obtained with the correlation coefficient ($r^2$) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and $7-96\;{\mu}g/kg$ in porcine muscle, and 4-32 and $13-97\;{\mu}g/kg$ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than $100\;{\mu}g/kg$.

Screening of Nitrosamine Impurities in Sartan Pharmaceuticals by GC-MS/MS

  • Chang, Shu-Han;Ho, Hui-Yu;Zang, Chi-Zong;Hsu, Ya-Hui;Lin, Mei-Chih;Tseng, Su-Hsiang;Wang, Der-Yuan
    • Mass Spectrometry Letters
    • /
    • v.12 no.2
    • /
    • pp.31-40
    • /
    • 2021
  • Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

Simultaneous Determination of Vitamin A and E in Infant Formula by HPLC with Photodiode Array Detection

  • Lee, Hong-Min;Kwak, Byung-Man;Ahn, Jang-Hyuk;Jeong, Seung-Hwan;Shim, Sung-Lye;Kim, Kyong-Su;Yoon, Tae-Hyung;Leem, Dong-Gil;Jeong, Ja-Young
    • Food Science of Animal Resources
    • /
    • v.31 no.2
    • /
    • pp.191-199
    • /
    • 2011
  • The objective of this study was to develop a method to simultaneously quantify vitamins A and E in infant formula. To determine the vitamin A and E content, vitamin A and four different vitamin E isomers (${\alpha}$-, ${\beta}$-, ${\gamma}$-, and ${\delta}$-tocopherol) were separated by high performance liquid chromatography with a photodiode array detector using a Develosil RPAQUEOUS RP-$C_{30}$ column ($4.6{\times}250$ mm, 5 ${\mu}M$). The vitamin A and E contents in the certified reference material determined using this method were within the certified range of standard values. The limits of detection (LODs) and limits of quantitation (LOQs) for vitamin A were 0.02 and 0.06 ${\mu}g/L$, respectively. LODs and LOQs for the vitamin E isomers ranged from 0.20 to 0.55 and from 0.67 to 1.81 ${\mu}g/L$, respectively. Linear analyses indicated that the square of the correlation coefficient for the vitamin A and E isomers was 0.9997-0.9999. The recovery of vitamins ranged from 96.69 to 97.79%. The results demonstrate that this novel method could be used to reliably analyze vitamin A and E content in infant formula.

Review of Rail Inspection Technology (철도 레일 결함 탐상기술 현황)

  • Han, Soon-Woo;Cho, Seung-Hyun
    • Proceedings of the KSR Conference
    • /
    • 2011.05a
    • /
    • pp.154-161
    • /
    • 2011
  • Rail inspection is very important as damages in rail can bring about a serious railway accident. In this paper, several real-time non-destructive technologies applied or considered to be applied to damage detection of rails are described. Some limits of existing ultrasonic testing method which has been widely used for rail inspection are discussed. Non-contact type NDE methods for rail inspection and their technical problems are also described.

  • PDF

A Solid-Phase Extraction Method for Analyzing Trace Amounts of Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans in Waste Water

  • Park, Deok-Hie;Youn, Yeu-Young;Choi, Jae-Won;Lim, Young-Hee;Cho, Hye-Sung
    • Mass Spectrometry Letters
    • /
    • v.2 no.1
    • /
    • pp.12-15
    • /
    • 2011
  • The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001.0.25 and 0.015.4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.

Assessment of total is ocyanates by OSHA and NIOSH analytical methods : accuracy and precision and airborne concentrations by process (NIOSH와 OSHA 측정 방법을 이용한 이소시아네이트류 발생 공정별 농도 분포 평가)

  • Kang, Hyoung Kyoung;Kim, Hyunwook
    • Journal of Korean Society of Occupational and Environmental Hygiene
    • /
    • v.9 no.2
    • /
    • pp.1-18
    • /
    • 1999
  • The purpose of this study was to compare performances of two analytical methods, the OSHA 42 and the NIOSH 5522, of quantifying total isocyanates in air. These methods were compared in terms of accuracy and precision and the detection limits using four(4) spiked samples in each of four(4) concentration levels which ranged from 0.25 to 2.0 times of the ACGIH TLV-TWA. In addition, two methods were used to as sess airborne concentrations of total isocyanates at the following processes including autobody spray painting, furniture spray painting, polyurethane foaming, urethane adhesion, UV coating, and pigment mixing. The results of this study showed that the NIOSH 5522 method was better than the OSHA 42 method in terms of accuracy, precis ion, and detection limit for quantifying airborne total isocyanates. It was also clear that the NIOSH method was capable of detecting not only monomeric but also non-monomeric isocyanates. The results of air concentrations of total isocyanates among processes studied indicate that some processes may exceed the recommended level of isocyanates. In addition, to evaluate toxicological effects of total isocyanates, it is recommended to consider additive effects of isocyanates present in mixtures.

  • PDF