• Title/Summary/Keyword: GC/MS spectrometry

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Identification of Aroma-Active Compounds in Korean Salt-Fermented Fishes by Aroma Extract Dilution Analysis 2. Aroma-Active Components in Salt-Fermented Shrimp on the Market (AEDA법에 의한 한국한 젓갈류의 Aroma-Active 성분의 구명 2. 시판 새우젓의 Aroma-Active 성분)

  • Cha, Yong-Jun;Kim, Hun;Jang, Sung-Min;Park, Jee-Young
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.28 no.2
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    • pp.319-325
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    • 1999
  • Volatile flavor compounds in Korean salt fermented shrimp on the market were analyzed by vacuum simultaneous distillation solvent extraction/gas chromatography/mass spectrometry/olfac tometry(V SDE/GC/MS/O) and aroma extract dilution anlaysis(AEDA). A total of 32 volatile com pounds were detected by GC/O analysis. Of these, 18 were positively identified, and composed of S containing compounds(5), aldehydes(4), ketones(3), N containing compounds(3), ester(1), alcohol(1) and aromatic hydrocarbon(1). Predominant odorants(Log3FD$\geq$4) in salt fermented shrimp were 2,3 butanedione(sour/buttery), 1 octen 3 one(earthy/mushroom like), dimethyl trisulfide(cooked cabbage /soy sauce like) and 2 acetylthiazole(grainy/nutty). Predominant free amino acids were aspartic acid, glutamic acid(sour and umami taste), arginine, methionine(bitter) and lysine(sweet and bitter) in evaluation of taste value.

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Volatile Flavor Compounds Derived from Anchovy Engraulis japonicus Sauce Residues through Maillard Reactions (멸치(Engraulis japonicus) 액젓 부산물로부터 마이야르 반응을 통해 유도 된 휘발성 향기성분)

  • Jin Hyeon Kim;Yong-Jun Cha;Daeung Yu
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.56 no.2
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    • pp.174-181
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    • 2023
  • Volatile flavor compounds of optimal Maillard reactions (MR) derived with the addition of precursors (AP), control (without AP) and raw as anchovy Engraulis japonicus sauce residue were identified and comparatively analyzed using solid phase microextraction/gas chromatography/mass spectrometry (SPME/GC/MS). MR was produced by adding 1% (w/w) glucose and mixed amino acids (threonine 0.543%, glutamic acid 0.194%, glycine 0.382%, w/w) to raw (100 g of anchovy sauce residue and 100 mL of distilled water), and heating at 110 ℃ for 2 h. Among 65 flavor components detected, 7 compounds were produced through Maillard reaction to change in content. A total of 7 volatile flavor compounds, including 2-methylbutanal, 3-methylbutanal, dimethyl disulfide, methylpyrazine, dimethyl trisulfide, methional, and 2-furanmethanol, tended to increase in the order of raw, control, and MR, but methylpyrazine was not detected in control. Amounts of 2-methylbutanal, 3-methylbutanal, dimethyl disulfide, methylpyrazine, dimethyl trisulfide, methional, and 2-furanmethanol having positive odors (dark chocolate-, garlic-, hazelnut-, cooked potato-like) were 11.04, 50.15, 3.25, 8.38, 4.60, 9.59, and 3.08 times higher, respectively, in MR than those in raw.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Determination of homogentisic acid in human plasma by GC-MS for diagnosis of alkaptonuria (GC-MS를 이용한 혈장 중 호모겐티식산의 분석;알캅톤뇨증의 진단)

  • Thapa, Maheshwor;Yu, Jundong;Lee, Wonjae;Islam, Fokhrul;Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.28 no.5
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    • pp.323-330
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    • 2015
  • Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Volatile Components of Traditional Gochujang Produced from Small Farms according to Each Cultivation Region (지역별 소규모 농가 생산 전통 고추장의 휘발성 성분에 관한 연구)

  • Hong, Yeo Joo;Son, Seong Hye;Kim, Ha Youn;Hwang, In Guk;Yoo, Seung Seok
    • Journal of the East Asian Society of Dietary Life
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    • v.23 no.4
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    • pp.451-460
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    • 2013
  • The purpose of this study is to investigate the volatile compounds of Korean traditional gochujang from various districts. The volatiles from each traditional gochujang are being extracted by simultaneous steam distillation extraction (SDE), and analyzed by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). Twenty compounds are identified as major volatile components which include 8 esters, 4 alcohols and 4 acids. The most traditional gochujang possesses more volatile components rather than commercial gochujang products. Most acids come from fatty acids and the alcohols derive from the oxidative degradation of linolenic acid. The most abundant volatile compounds for both traditional and commercial gochujang include 10 compounds such as 2-methyl-1-propanol, hexanal, 2-methyl-1-butanol, octanoic acid ethyl ester, as well as the various type of acids and esters. They represent most of the total GC peak areas, respectively. From the results, the characteristics of the flavors for traditional gochujang from each district are not clear but have shown various components than the commercial products.

Changes of Volatile Components of Pleurotus sajor-caju During Storage (여름 느타리 버섯 (Pleurotus sajor-caju) 저장중의 향기성분 변화)

  • Jung, Soon-Taek;Hong, Jai-Sik
    • The Korean Journal of Mycology
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    • v.19 no.4
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    • pp.292-298
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    • 1991
  • Volatile aroma concentrates of Pleurotus sajor-caju which stored at $20^{\circ}C$ incubator and cold room were obtained by simultaneous distillation-extraction method. The volatile components were identified by combined capillary gas chromatography-mass spectrometry and comparison of retention data on GC of those authentic compounds. Storage at room temperature resulted in significant decreased in their total aroma contents, whereas little changes at cold storage foured, even though appreciable changes were observed in GC pattern between the control and stored samples. Of 38 components identified, ${\delta}-decalactone$ increased while rest of the volatiles decreased rapidly during storage at room temperature, but at cold storage 2-methyl butanal, 1-octen-3-ol, cis,cis-1,5-octadien-3-ol and pentadecanoic acid decreased while 3-octanone, 1-octen-3-one, 3-octanol and 5-undecanol increased with the storage time. The weight losses and organoleptic properties changed extremely by the storage under room temperature, on the other hand, slight changes were found in cold storage.

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An Identification of Volatile Terpenes in Allelopathic Weeds (Allelopathy 작용성(作用性)을 나타내는 잡초(雜草)중의 휘발성(揮發性) Terpene류(類)의 동정(同定))

  • Chun, J.C.;Han, K.W.
    • Korean Journal of Weed Science
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    • v.9 no.2
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    • pp.149-153
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    • 1989
  • Volatile terpenes responsible for allelopathic activity in four weed species were identified using gas chromatography (GC) and GC-mass spectrometry. Artemisia asiatica Nakai contained 26 volatile terpenes, consisting of 16 monoterpenes and 10 sesquiterpenes, whereas there were only four terpenes in Trifolium repens L. and three terpenes each in Portulaca oleracea L. and Capsella bursa-pastoris (L,) Medik. Suspected allelochemics were ${\alpha}$-phellandrene, 1,8-cineole, limonene, ${\alpha}$-pinene, borneol, selinene, and caryophyllene in A. asiatica, ${\alpha}$-pinene and ${\beta}$-caryophyllene in T. repens, and ${\alpha}$-pinene in C. bursapastoris. No these compounds were found in P. oleracea.

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Studies on the Free and Bound Aroma Compounds in Green and Fermented Teas (녹차와 후발효차의 유리형 및 결합형 향기성분에 대한 연구)

  • Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.43 no.4
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    • pp.407-412
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    • 2011
  • Free and bound aroma compounds in green and fermented teas treated with microbial-fermentation were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. Aldehydes and ketones in green tea decreased during microbial fermentation, whereas linalool and geraniol increased in the fermented tea. After enzyme treatment, (Z)-3-hexen-1-ol increased significantly following enzymatic hydrolysis of both green and fermented teas. In addition, benzaldehyde, 3-hexenyl acetate, and geraniol also increased in green tea with enzyme treatment. Bound aroma compounds in the green and fermented teas increased at different levels of added enzyme. We demonstrated the enhancement of both green and fermented teas by enzyme treatment, which can lead to improvement in the flavor qualities of green and fermented teas.