• Title/Summary/Keyword: selected ion monitoring

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Analysis of Ginsenosides by Thermospray LC/MS (열분무 LC/MS에 의한 인삼사포닌의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Hwang, Gwi-Seo;Lee, Mi-Young;Park, In-Jeong
    • Journal of Ginseng Research
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    • v.19 no.2
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    • pp.134-137
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    • 1995
  • Ginseng saponins were analyzed by thermospray (TSP) LCMS method using ODS column and with acetonitrile/ammonium acetate solution. Optimal condition for TSP Lchfs was found as follows: capillary temperature: 33$0^{\circ}C$ repelled voltage: 200 V, and concentration of ammonium acetate: 0. 05 M. Panaxadiol and panaxatriol type saponins showed characteristic fragment ions. The calibration curve of ginseng saponin showed good linearity with a correlation coefficient of 0.99. Detection limits using selected ion monitoring (SIM) technique were improved by 10~200 times compared to conventional HPLCnnr detection method.

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Research for the Analytical Method of Various Pesticides in Raw Milk by Gas Chromatography-Mass Spectrometry (GC/MSD를 사용한 원유 내 잔류농약의 분석법 연구)

  • Oh, N.S.;Shin, Y.K.;Baick, S.C.
    • Food Science of Animal Resources
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    • v.29 no.4
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    • pp.482-486
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    • 2009
  • The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

Analysis of Residual Pesticides in Herbal Drugs: GC/MS Analysis of 27 Controlled Pesticides (생약 중 잔류 농약의 분석법: GC/MS에 의한 27종 잔류 규제 농약의 분석)

  • Park, Man-Ki;Park, Jeong-Hill;Yoon, Hye-Ran;Yoon, In-Byoung;Cho, Sool-Yeon;Hwang, Gwi-Seo
    • YAKHAK HOEJI
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    • v.40 no.2
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    • pp.141-148
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    • 1996
  • GC/MS analysis of 27 controlled pesticides in herbal drugs was studied. Selected ion monitoring(sim) technique was applied to increase the GC/MS sensitivity. Typical peaks in th e mass spectrum of each pesticides were selected as quantitation, comfirmation or alternate ion. Twenty seven pesticides were divided into five groups according to their retention time and the peaks for SIM were programmed accordingly. The combination of two ionization methods, electron impact(EI)-SIM-MS and negative ion chemical ionization(NCI)-SIM-MS, were well-fitted for the detection, confirmation and quantitation of multiclass residual pesticides in herbal drugs.

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Development of Real-time and Simultaneous Quantification of Volatile Organic Compounds in Ambient with SIFT-MS (Selected Ion Flow Tube-Mass Spectrometry) (선택적다중이온질량분석기를 이용한 대기 중 휘발성유기화합물 실시간 동시분석법 개발 및 적용)

  • Son, Hyun Dong;An, Joon Geon;Ha, Sung Yong;Kim, Gi Beum;Yim, Un Hyuk
    • Journal of Korean Society for Atmospheric Environment
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    • v.34 no.3
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    • pp.393-405
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    • 2018
  • Volatile organic compounds (VOCs) are representative air pollutants due to their detrimental effects on human health and their role in formation of secondary organic aerosols. Assessments and monitoring programs of VOCs using periodic grab sampling like Tedlar bags, canisters, and sorbent traps provide limited information, often with delay times of days or weeks. Selected ion flow tube mass spectrometry (SIFT-MS) is an emerging analytical technique for the real-time quantification of VOCs in air. It relies on chemical ionization of the VOCs molecules in air introduced into helium carrier gas using $H_3O^+$, $NO^+$, and $O_2{^+}$ precursor ions. Real-time monitoring method of 60 VOCs in the ambient air was developed using TO-15 standard gas mixture. Calibration curves, method detection limit, and quantitation reproducibility of the target compounds were tested. Dynamic dilution system was used to dilute standard gas from 0.174 ppbv to 100 ppbv, where calibration curves showed good linearity with $r^2$> 0.95 in all target analytes. Limit of detection (LOD) all compounds were sub ppbv, and some halogenated compounds showed pptv levels. Seven consecutive analyses of target compounds showed good repeatability with relative standard deviation of less than 10%. One day monitoring of VOCs in ambient air was conducted in Geoje. Average concentration of target VOCs in Geoje were relatively lower than other regions, among which formaldehyde showed the highest concentration ($15.4{\pm}5.78ppbv$). SIFT-MS provided good temporal resolution data (1 data per 3.2 minute), which can be used for identifying ephemeral short-term event. It is expected that SIFT-MS will be a versatile monitoring platform for VOCs in ambient air.

Simultaneous Determination of Asperosaponins and Iridoid Glycosides from Dipsaci Radix by Using LC-ESI-MS Spectrometry (속단(Dipsaci Radix) 중 Asperosaponins 및 Iridoid glycosides의 LC-ESI-MS에 의한 동시분석)

  • Cho, Hwang-Eui;Son, In-Seop;Kim, Sun-Cheun;Son, Kun-Ho;Woo, Mi-Hee;Moon, Dong-Cheul
    • Korean Journal of Pharmacognosy
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    • v.43 no.2
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    • pp.137-146
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    • 2012
  • Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

Analysis of Flavor-related Compounds from Tobacco using SPME-GC-MS (SPME-GC-MS를 이용한 담배와 관련된 향료의 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.109-114
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    • 2001
  • The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry(GC-MS). Flavor-related compounds were estragole pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin. More than on of the flavor-related compounds were detected in the range $0.001-1.3{\mu}g/g$ from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%.

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Simultaneous determination of parabens in cosmetics by LC/MS (LC/MS를 이용한 화장품 중의 parabens 동시 분석 방법 연구)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.54-59
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    • 2010
  • The simultaneous analysis of parabens in cosmetic samples was carried out by LC/MS. The cosmetic samples are directly dissolved in methanol and filterated using $0.45\;{\mu}m$ filter. The methanol-water was used for the mobile phase of gradient conditions. An Extend $C_{18}$ reverse-phase column and the selected ion monitoring (SIM) mode were applied. The analysis results of LC/MS showed good linearity with correlation coefficient of $r^2$=0.9993 in the range of 0.05 to $10\;{\mu}g$/mL and detection limit of $0.01\;{\mu}g$/mL.

Sensitive Determination of Alkylphenols, Chlorophenols, and Bisphenol A using GC/MS-SIM in Paper Materials (기체 크로마토그래피/질량분석기를 이용한 종이류 중 알킬페놀류, 클로로페놀류 및 비스페놀 A 정량)

  • Kim, Hyub;Kim, Jin-Ho
    • Environmental Analysis Health and Toxicology
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    • v.18 no.1
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    • pp.45-55
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    • 2003
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid -phase extraction (SPE) with XAD -4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8%) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 ng/g in 2,4-dichlorophenol, 1.01 ∼ 1.17 ng/g in t-butylphenol,2.17 ∼ 5.84 ng/g in pentachlorophenol, 12.68 ∼ 14.88 ng/g in nonylphenol and 30.84 ∼ 153.72 ng/g in bisphenol A.