• Title/Summary/Keyword: ID-GC-MS

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Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 오미자 Lignan성분의 동정)

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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Development of Simultaneous Analysis for Multiple Agricultural Pesticides in Raw Milk Products using GC-MS/MS (GC-MS/MS를 이용한 원유 원료 중 농약 동시분석법 확립)

  • Young Nae Choi;Yoon ho Shin;Hwangeui Cho;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.420-429
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    • 2023
  • GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

Quantitative Analysis of Isoflavones and Lignans in Sea Vegetables Consumed in Korea Using Isotope Dilution Gas Chromatography-Mass Spectrometry

  • Lee, Young-Joo;Adlercreutz, Herman;Kwon, Hoon-Jeong
    • Food Science and Biotechnology
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    • v.15 no.1
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    • pp.102-106
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    • 2006
  • The phytoestrogens including isoflavones (genistein, daidzein, biochanin A, formononetin, and glycitein), coumestrol, and lignans (secoisolariciresinol, matairesinol, and anhydrosecoisolariciresinol) were quantified in edible sea vegetables from Korea. Sea vegetable samples were collected based on domestic consumption data. After hydrolysis of phytoestrogen glycosides in prepared samples, aglycones of phytoestrogens were extracted with diethyl ether and analyzed with isotope dilution gas chromatography-mass spectrometry in selected ion monitoring mode (ID-GC-MS-SIM). Total samples included 19 samples representing eight species. Most of the samples showed rather low concentrations, ranging from not determinated to $79.2\;{\mu}g/kg$ for isoflavones and from 106.4 to $694.8\;{\mu}g/kg$ for lignans. The daily intake of phytoestrogen from sea vegetables, estimated from the present data and domestic consumption data, was about $0.13\;{\mu}g/day$ for isoflavones and $2.0\;{\mu}g/day$ for lignans. When we compared these results with those from legumes, sea vegetables would not be considered the major source of phytoestrogens in the Korean diet.

Determination of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Capillary-GC(FID) (Capillary-GC(FID)에 의한 오미자 Lignan 성분의 정량)

  • Sohn, Hyun-Joo;Bock, Jin-Young;Baik, Soon-Ok;Kim, Yong-Ha
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.350-356
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    • 1989
  • The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

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Electromyographic and Biomechanical Analysis of Postural Movement Patterns During the Backward Sway (Backward Sway 동안의 자세움직임 형태에 대한 근전도와 생체역학적 분석)

  • You, Sung-Hyun
    • Physical Therapy Korea
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    • v.2 no.2
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    • pp.1-8
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    • 1995
  • 이 논문의 주목적은 정상인을 대상으로 각기 다른 3가지의 (체중의 1.5 %, 3.0 %, 9.0 %) 부하를 통해서 자세의 불균형을 유발시켰을 때 나타나는 postural movement patterns을 기술하기 위한 연구이다. 연구대상의 허리중심에 체중부하를 주어 균형이 뒤로 이동하게 하여, surface EMG(표면 근전도)를 통하여 Tibialis anterior(Ta), Gastrocnernius(Gc), Quadriceps femoris(Qc), Hamstring(Ha), Rectus abdominalis(Ab)와 Paraspinalis(Pa) 근육들의 motor recruitment pattern(운동회집형태)를 측정하였다. 그리고 비디오 촬영은 고관절, 슬관절, 족관절의 움직임을 보기 위해 사용하였다. 특히 근전도 (EMG)는 자세반응 검사에 있어 첫 근반응(근수축) 경과시간(FR)과 분절간격간의 (ID)시간을 조사하는데 사용되었다. 이 연구의 결과는 4가지 중요한 사실을 전해주고 있다. 첫 번째로서, 연구대상자에게 체중의 1.5 %의 부하를 적용하였을 때 Ta가 가장 먼저 수축을 시작하였고(FR:$88{\pm}19.4$ ms) 발목과 대퇴사이의 분절 간격간(ID)의 평균은 +9.3 ms였다. 또한 족관절의 변화가 가장 뚜렷하여 Nashner(1985)의 족기전을 뒷받침하고 있다. 둘째로는 연구대상자에게 체중의 3.0 %의 부하를 주었을 때 Qc와 Ab근육이 원위부에서 근위부 순서로 수축하였고, 첫 번째 근육수축시간은 ($82{\pm}39.2$ ms)였다. 그리고 이때 분절간격의 평균은 +8.3ms 이였고 Ta는 거의 반응하지 않았다. 족관절과 슬관절에 비해 고관절의 변화가 가장 현저하게 나타났고, 이 또한 Nashner의 고관절 기전과 같은 현상을 보였다. 셋째로 연구 대상자에게 체중의 9.0 % 부하를 허리에 적용하였을 때 근수축은 근위부에서 원위부 순서를 이루어졌다. 즉 Ab,Qc, Ta, Ps순으로 근수축 되었다. Ab가 처음으로 수축하여 첫 반응(FR)은 $73{\pm}3.2$ ms 이였고 슬관절과 고관절의 변화가 가장 뚜렷하였다. 넷째로 연구 대상자에게 체중의 9.0 %부하를 적용하였을 때, 균형을 잡기 위해 뒷걸음치는 것이 관찰되었고 이때 근수축 순서는 Ta,Ab.Ps,Qc,Hs였다. 이 결과는 Nasher의 결과와 불일치하였다. 이상과 같은 결과에서 연구대상자의 자세운동형태(postural movement patterns)는 각기 다른 부하 정도와 시간에 따라 합성적으로 이루어지는 것으로 보여졌다. 특히, 자세운동형태는 부하의 적용위치와 연구대상자의 최근의 경험에 영향을 받은 것으로 밝혀졌다. 결론적으로 말하면 자세운동형태는 중앙신경계의 제한적(한정적) 명령 시스템에 의해서 움직임(movement)이 발생하기 전에 조직된다는 Nashner의 가설을 뒷받침하였다.

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Comparison of QuEChERS and Solid Phase Extraction for Accurate Determination of Pesticide Residues in Kimchi Cabbage and Strawberry using Isotope Dilution Mass Spectrometry

  • Seonghee Ahn;Kebede Gebeyehu Mekete;Byungjoo Kim
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.178-185
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    • 2023
  • QuEChERS is used worldwide as a universal sample preparation method with many benefits, such as being quick, easy, cheap, effective, rugged and safe. This study examined whether QuEChERS can be employed in isotope dilution mass spectrometry (ID-MS) for accurate analysis of pesticides in food. The ratios of fortified values and measured values of malathion and fenitrothion using the QuEChERS method were compared with those using the solid phase extract (SPE) method which was previously used in this laboratory. The separations of the two pesticides on DB-5MS and VF-1701MS columns were compared. Malathion and fenitrothion were fortified into kimchi cabbage and pretreated with the QuEChERS method and the SPE method. The results obtained using the DB-5MS column varied according to the sample preparation method, column and pesticide level. Using the VF-1701 column, ratios were 98-102% by both QuEChERS and Carb/NH2 SPE method for all fortification level. Malathion and fenitrothion were fortified into strawberry samples for comparison with kimchi cabbage. The results for the strawberry samples indicated that the ratios were not influenced by the sample preparation methods or GC column. The QuEChERS method could be acceptable in the ID-MS method for pesticide residue analysis in food, however other conditions should be carefully considered for accurate determination, such as the column, amount of analyte and food matrix.

A study on the development of phthalate plasticizers CRM in ABS resin (ABS 중 phthalates 가소제 CRM 개발에 대한 연구)

  • Jung, Jung-Sul;Park, Jung-Woo;Yoo, Seok;Kweon, Seong-Il;Hong, Sung-Taeg;Sun, Yle-Shik;Park, Cheon-Min;Choi, Chang-Hyoo
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.273-283
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    • 2012
  • Phthalate plasticizers are regulated by RoHS, REACH and CPSC as hazardous substances. Responding to these international environmental restrictions, we developed ABS certified reference material (CRM) for determination of phthalate plasticizers such as DMP, DEP, DBP, BBP, DEHP and DnOP. The candidate material has been made with ABS resin widely used in electric and electronic products and 6 kinds of phthalate plasticizers. The making of the material involved a series of processes like extruding, cooling, pelletizing, and drying using twin screw extruder. Then it has been certified according to ISO Guide 35. Using isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS), homogeneity, short-term stability, and long-term stability were evaluated. The certified values were determined by using primary reference material (PRM) of KRISS for traceability. From now on, we will provide ABS CRM to national and international companies and research institutes after certification as certified reference material and registering on COMAR (code of reference material).

Trans Fatty Acid Isomers of Processed Foods Commonly Consumed in Korea (한국인 상용 가공식품의 trans 지방산 이성체)

  • 노경희;원미숙;송영선
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.3
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    • pp.325-337
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    • 2003
  • This study was designed to determine the distribution of trans fatty acids (tFAs) isomers of Processed foods commonly consumed in Korea. The tFAs positional isomers were analyzed using GC/MS spectrometer with HP-23 cis/trans FAME, capillary column (50m $\times$ 0.20 mm, id., 0.2 ${\mu}{\textrm}{m}$ film thickness) for 41 food samples. TFAs isomers were identified by comparing retention time with standards and GC/MS spectrum. In margarines, the content of tFAs ranged from 4.0% to 25.16% and the most abundant positional isomer of tFAs was C18:1 $\Delta$9t. In oils and fats, lards contained higher levels of tFAs (5.70~16.54%) than shortenings (6.77~10.55%). Shortenings contained higher levels of C18:1 $\Delta$9t (3.1~5.1%) than lard (1.6~4.3%), but corn oils had no tFAs. In seasonings, mayonnaise had no C16:1 $\Delta$9t, whereas C18:3t was detected. The content of tFAs in confectioneries was wide (16.20~52.16%). Among them, instant popcorns contained the highest amount of tFAs. Milk and dairy products showed even distribution of tFAS such as C18:1t, C18:2t, and C18:3t. Predominant tFAS isomer of condensed milk and ice cream was C16:1 $\Delta$9t. Frozen french fries and fried chicken contained higher levels of C18:1$\Delta$9t (9.4%), whereas grilled pork (jowl) had no C18:1 $\Delta$9t. The amount of tFAs per serving size was the highest in popcorn, followed by frozen pizza, frozen french fries, fried chicken, and bakeries.

Characterization of Product Gas and Residues from Arc Cracking of Waste Lubricating Oil (폐윤활유의 아크 열분해 생성물 및 잔류물 특성 연구)

  • 김인태;김정국;송금주;서용칠;김준형
    • Resources Recycling
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    • v.8 no.5
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    • pp.34-43
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    • 1999
  • An elecmc arc cracking reaclor is developed for the productiol~o f ieusuble fuel gas by the thennal destruction of waste oil. The churaclensucs of product gas and ~esiduesf rom arc crachng of wnste lubr~cat~nogil are sludird. Thc product gas is mainly coruposcd of hydrogen 135-4076), acetylene (13-4076), ethylene 13-476) and olher hgdrocnrbons. The contenr of carbon monomde, one or the main product in a conventional low-temperature Lhennal cracking umt, 1s very slnvll in lhis atc cracking expcnmcnt. Total calocctic wlue of product gas shows 11,000-13.000 kcizlkg, which is hiph cnough to use as a ~ L I I I Cga~ s . and the concentralions oC loxic gases arc well below the rcguliltury emission critena The GCIMS analysis of llquld-phase residues shows that the high rnalccular welgllt hydrocilrbons in the waste oil arc cracked into the low malecular weight hydrocarbons snd hydroem,. The dehydrogcnntion is found lo be Lhe main cracking rcacuon due lo the high temperalure ~ ~ ~ d ubcyc edle ctric arc. The average parucle size of soot as the solid-phase residue is 10 3 wm, and the conlents of cabon a ~ hdea vy metals are abovc 60% and under 0.01 ppm, respecttrely. Thc utllizvtion or sool, as industl-id1 rcsource seems lo he reasible aIter refimng.

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