• Title/Summary/Keyword: Method detection limits

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Determination of Selenium and Tellurium by HG-AAS in Foods

  • Cha, Ki-Won;Park, Sang-Ho;Park, Kwang-Won
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.419-425
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    • 1995
  • A method has been investigated for the determination of selenium and tellurium in Ginseng, Ganoderma and Garlic using hydride generation atomic absorption spectrometry(HG-AAS). The concentration effects of hydrochloric acid and sodium tetrahydroborate on the hydride generation for the determination of selenium and tellurium were investigated. The method of sample decomposition was also investigated using various mineral acids, such as nitric, perchloric and sulfuric acid in the closed system, and foreign ion effects containing in the samples were studied. The calibration curves of selenium and tellurium were obtained in the range of 0~40 ppb. The detection limits(S/N=2) of selenium and tellurium are 0.1 and 0.2 ppb. Analytical data of selenium and tellurium in Garlic, Ganoderma and Ginseng are 289, 296 and 198 ng/g for selenium and 146, 127 and 110 ng/g for tellurium, respectively.

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Studies on the Comparison of Scutellaria Radix Analyses by CE and HPLC (모세관전기영동장치 및 고속액체 크라마토그래피에 의한 황금의 성분 분석법 비교)

  • 면노홍;김효진
    • YAKHAK HOEJI
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    • v.43 no.4
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    • pp.429-436
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    • 1999
  • A simple, accurate and reproducible Capillary electrophoresis (CE) assay has been developed for the determination of baicalin, baicalein, wogonin and chrysin in Scutellaria baicalensis. Successful separation of these compounds has been obtained in 35 mM phosphate butter (pH 7.0) using a untreated fused silica capillary ($57{\;}cm{\times}75{\;}{\mutextrm{m}}$ i.d.) at $25^{\circ}C$ with the electric field of 19kV. Baicalin, baicalein wogonin and chrysin was separated and detected at 280 nm 13 min. The detection limits of CE were acceptable compared to HPLC. Reproducibilities of migration time and peak area were 0.66~1.11% (within-run), 2.18~3.38% (between-run) and 3.50~4.55% (within-run), 3.97~4.82%(between-run) at CE. The results indicate that CE could be a promising technique for quality and quantity control analysis of Scutellaria baicalensis as a validation method.

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The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque (고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법)

  • Ahn Sang-Woo;Lee Si-Jin;Chang Soon-Woong
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.

Determination of Icing Inhibitors (Ethylene Glycol Monomethyl Ether and Diethylene Glycol Monomethyl Ether) in Ground Water by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Jung, Dong-Gyun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.806-808
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    • 2004
  • A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of icing inhibitors, ethylene glycol monomethyl ether and diethylene glycol monomethyl ether in ground water contaminated with JP-8. Ethylene glycol monobutyl ether and ethylene glycol monoethyl ether were used as the internal standard and surrogate, respectively. 100 mL of ground water was extracted twice with 20 mL of methylene chloride. The extract was concentrated to dryness, dissolved with 100 ${\mu}$L of methanol and analyzed by GC-MS (SIM). The use of an Innowax column gave the peaks good chromatographic properties, and the extraction of these compounds from samples gave recoveries of about 50% with small variations. The method detection limits of the target compounds were in a range of 0.5-0.8 ng/mL in ground water.

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.

Determination of Liraglutide in Rat Plasma Using Selective Liquid Chromatography-Tandem Mass Spectrometry

  • Younah Kim;Hyoje Jo;Yelim Lee;Soo Yeon Kang;Sangkyu Lee
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.141-146
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    • 2023
  • Liraglutide is a medication prescribed for the management of type 2 diabetes and chronic obesity. A simple, sensitive, and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitative analysis of liraglutide in rat plasma. After a simple protein precipitation step, liraglutide was chromatographically separated using the ACQUITY Premier Peptide BEH C18 Column with mobile phases comprising 50% acetonitrile and 50% methanol, and water with 0.3% FA. Positive ion electrospray ionization in multiple reaction monitoring mode was used to achieve detection. Good linearity was observed in the 5-600 ng/mL concentration range (R2 > 0.99). Liraglutide had intra- and inter-day precision values of 2.13%-9.86% and 4.14%-8.36%, respectively. The accuracy ranged from -2.36% to 2.58%. The recovery and matrix effect were within acceptable limits. This selective LC-MS/MS method was used to study the pharmacokinetic properties of liraglutide after subcutaneous administration in rats.

Development of a Simultaneous Detection and Quantification Method of Anorectics in Human Urine Using GC-MS and its Application to Legal Cases (GC-MS를 이용한 사람 뇨시료 중 비만치료제 분석 및 비만치료제 남용 현황의 법과학적 고찰)

  • Choi, Hyeyoung;Lee, Jaesin;Jang, Moonhee;Yang, Wonkyung;Kim, Eunmi;Choi, Hwakyung
    • YAKHAK HOEJI
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    • v.57 no.6
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    • pp.420-425
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    • 2013
  • Phentermine (PT) and phenmetrazine (PM) have been widely used as anti-obesity drugs. These drugs should be used with caution due to its close relation to amphetamine in its structure and toxicity. PT and PM, amphetamine-type anorectics, have recently been considered as alternatives for methamphetamine abuse in Korea. In addition, the misuse and abuse of PT and PM obtained by illegal sources such as the internet become a serious social problem. In the present study, a simultaneous detection and quantification method for determining PT and PM in human urine was developed and validated according to the international guidelines. The urine samples were screened using a fluorescence polarization immunooassay and analyzed by gas chromatography mass spectrometry (GC-MS) after extraction using automatic solid phase extraction (SPE) with a mixed-mode cation exchange cartridge and derivatization with pentafluoropropionic anhydride (PFPA). The validation results for selectivity, linearity, limits of detection (LOD) and quantification (LOQ), intra- and inter-assay precision and accuracy and recovery were satisfactory. The validated method was successfully applied to authentic urine samples collected from 38 drug abuse suspects. PT and/or PM were identified with or without methamphetamine in urine samples. Abuse of PT and PM have increased continuously in Korea, therefore, closer supervision of the inappropriate use of anoretics is necessary.

The Comparison Study in the Extraction of Inorganic Priority Pollutants from Solid Wastes (고체 폐기물 시료 중의 무기 Priority Pollutants 추출법 비교 연구)

  • Ahn, Tae-Ho;Lee, Huk-Hee;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.395-402
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    • 1997
  • The comparison study between EPA method 3050 and the test method offered by Ministry of Environment in Korea was performed to investigate a matrix effect on extraction. In this study, 12 inorganic priority pollutants(Cd, Cr, Cu, Pb, Ni, Zn, As, Sb, Se, Hg, Be, Tl) were spiked to the sludges and estuary sediment samples. The extracts were analyzed by AAS, HG-AAS, and ICP/MS. Results were discussed in terms of recoveries, relative standard deviations, and the method detection limits. Mean recovery of the elements except As, Sb, and Se was 93% when the procedure of EPA method was applied. The Korean extraction method, however. showed a significant matrix effect to give very poor recoveries.

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Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

Comparison of Analytical Methods for the Detection of Paralytic Shellfish Toxins (PSTs) (마비성패류독소 검출을 위한 분석법 비교)

  • Lee, Ka Jeong;Kwon, Soon Jae;Jung, Yeoun Joong;Son, Kwang Tae;Ha, Kwang Soo;Mok, Jong Soo;Kim, Ji Hoe
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.50 no.6
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    • pp.669-674
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    • 2017
  • Paralytic shellfish toxins (PSTs) are produced by marine dinoflagellate phytoplankton Alexandrium spp. and Gymnodinium spp. These toxins accumulate in filter feeding organisms such as bivalves and the ingestion of contaminated shellfish can cause illness in humans. The mouse bioassay (MBA) has been the preferred PST testing method worldwide for more than 50 years. However, this assay has several disadvantages, such as detection limits, non-toxic-profiles, and the ethical issues of using animals. The aim of this study was to establish an alternative to the MBA method for testing for PSTs. We optimized the analysis conditions of a post-column oxidation-high performance liquid chromatography (PCOX-HPLC) method and the Scotia Rapid Test Kit, and then compared the accuracy of these methods to the MBA method. The results demonstrated a strong correlation between the PCOX-HPLC method and the MBA, although the PCOX-HPLC method required expensive equipment and standard material, and was time consuming. The Scotia Rapid Test Kit promises to be a useful tool, as it provided rapid and qualitative results, although the method sometimes gave a false positive result that could not be explained by toxin profiles.