• Title/Summary/Keyword: gas chromatography/mass spectrometry (GC/MS)

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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).

Monitoring of Uniconazole by GC-NPD (GC-NPD 동시분석법을 이용한 유니코나졸 잔류실태조사)

  • Kim, Eun-Jeung;Choi, Bu-Chuhl;Choi, Su-Jeong;Hong, Chae-Kyu;Kim, Eun-Hee;Choi, Chae-Man;Seo, Young-Ho;Hwang, Young-Sook;Jang, Mi-Ra;Hwang, In-Sook;Kim, Moo-Sang;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.378-381
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    • 2012
  • The monitoring of the uniconazole residual pesticide for agricultural products was conducted by multiclass pesticide multiresidue methods. Samples were collected from June to November, 2011. Uniconazole pesticide was detected in 49 samples from a total of 3,939 samples. The amount of uniconazole pesticide ranged from 0.09 to 17.89 mg/kg in 49 samples. This method was described for the simultaneous determination of uniconazole by gas chromatography with a nitrogen phosphorus detector (GC-NPD) and mass spectrometry (MS). The limit of detection and quantification were 0.006 and 0.018 mg/kg GC-NPD, respectively. For an evaluation of the GC-NPD method, uniconazole spiked into gyeojachae at a level of 0.5, 5 mg/kg was determined. The recoveries of uniconazole by the GC-NPD method ranged from 83.4 to 101.4%. The results indicate that the method of simultaneous analysis is applicable to uniconazole analysis.

The Factors for the Formation of Carcinogenic N-Nitrosamine from Dried Marine Food Products (수산 건제품중 발암성 N-NITROSAMINE의 생성 요인)

  • SUNG Nak-Ju;KANG Shin-Kwon;LEE Soo-Jung;KIM Sung-Hee
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.27 no.3
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    • pp.247-258
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    • 1994
  • A total of 31 commercial dried marine food products, consisting of 14 fishes, 2 shellfishes and 2 seaweeds species were analyzed for their contents of precusors of N-nitrosamine such as dimethylamine(DMA), trimethylamine(TMA), trimethylamine oxide (TMAO), betaine and nitrate and nitrite nitrogen as factors of N-nitrosamine formation. Carcinogenic N-nitrosamines were extracted by a steam distillation apparatus and were analyzed for their components using a gas chromatography-thermal energy analyzer. N-nitrosodimethylamine(NDMA) was confirmed by a gas chromatography-mass spectrometry. The contents of betaine nitrogen in samples were in the range of $5.2{\sim}373.8mg\%$ and were significantly higher than tertiary amines such as TMA and TMAO. DMA nitrogen in those samples was in the range of trace-31.2ppm and was high, in the dried shark(31.2ppm), alaska pollack($22.9{\sim}24.3ppm$) and octopus($17.9{\sim}18.4ppm$). In dried laver and sea mustard, however, amines were not detected at all. The levels of nitrate nitrogen in the dried marine samples ranged from zero to 16.8ppm and were high in the dried stingray(16.8ppm), alaska pollack(16.3ppm) and squid($2.2{\sim}12.4ppm$), but were less than 1.0 ppm in other samples. The levels of nitrite nitrogen were lower than those of nitrate nitrogen and it was not detected in dried sea cucumber, laver and sea mustard. Twenty eight of 31 samples contained NDMA($range=1.2{\sim}86.0ppb$), which was the only volatile N-nitroso compound found. The NDMA levels of dried stingray($2.8{\sim}86.0ppb$), alaska pollack($8.2{\sim}55.5ppb$), squid($3.3{\sim}53.2ppb$), yellow corvenia($45.9ppb$) and plain dried shrimp($15.4{\sim}17.9ppb$) were high. However, it was not detected in dried sea cucumber, laver and sea mustard. Samples, containing high levels of NDMA, also contained high nitrate and nitrite nitrogen. From above results, it can be concluded that nitrate and nitrite were major factors for the formation of NDMA in dried marine food products.

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Antibacterial, Anti-Diarrhoeal, Analgesic, Cytotoxic Activities, and GC-MS Profiling of Sonneratia apetala (Buch.-Ham.) Seed

  • Hossain, Sheikh Julfikar;Islam, M Rabiul;Pervin, Tahmina;Iftekharuzzaman, M;Hamdi, Omer AA;Mubassara, Sanzida;Saifuzzaman, M;Shilpi, Jamil Ahmad
    • Preventive Nutrition and Food Science
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    • v.22 no.3
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    • pp.157-165
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    • 2017
  • Fruits of Sonneratia apetala (Buch.-Ham.), (English: mangrove apple, Bengali: keora) both seeds and pericarps, are largely consumed as food besides their enormous medicinal application. The fruit seeds have high content of nutrients and bioactive components. The seeds powder of S. apetala was successively fractionated using n-hexane, diethyl ether, chloroform, ethyl acetate, and methanol. The fractions were used to evaluate antibacterial, anti-diarrhoeal, analgesic, and cytotoxic activities. Methanol fraction of seeds (MeS) stronly inhibited Escherichia coli strains, Salmonella Paratyphi A, Salmonella Typhi, Shigella dysenteriae, and Staphylococcus aureus except Vibrio cholerae at $500{\mu}g/disc$. All the fractions strongly inhibited castor oil induced diarrhoeal episodes and onset time in mice at 500 mg extract/kg body weight (P<0.001). At the same concentration, MeS had the strongest inhibitory activity on diarrhoeal episodes, whereas the n-hexane fraction (HS) significantly (P<0.05) prolonged diarrhoeal onset time as compared to positive control. Similarly, HS (P<0.005) inhibited acetic acid induced writhing in mice at 500 mg extract/kg, more than any other fraction. HS and diethyl ether fractions of seed strongly increased reaction time of mice in hot plate test at 500 mg extract/kg. All the fractions showed strong cytotoxic effects in brine shrimp lethality tests. Gas chromatography-mass spectrometry analysis of HS led to the identification of 23 compounds. Linoleic acid (29.9%), palmitic acid (23.2%), ascorbyl palmitate (21.2%), and stearic acid (10.5%) were the major compounds in HS. These results suggest that seeds of S. apetala could be of great use as nutraceuticals.

Chemical Vapor Deposition of Ga2O3 Thin Films on Si Substrates

  • Kim, Doo-Hyun;Yoo, Seung-Ho;Chung, Taek-Mo;An, Ki-Seok;Yoo, Hee-Soo;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.23 no.2
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    • pp.225-228
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    • 2002
  • Amorphous $Ga_2O_3$ films have been grown on Si(100) substrates by metal organic chemical vapor deposition (MOCVD) using gallium isopropoxide, $Ga(O^iPr)_3$, as single precursor. Deposition was carried out in the substrate temperature range 400-800 $^{\circ}C$. X-ray photoelectron spectroscopy (XPS) analysis revealed deposition of stoichiometric $Ga_2O_3$ thin films at 500-600 $^{\circ}C$. XPS depth profiling by $Ar^+$ ion sputtering indicated that carbon contamination exists mostly in the surface region with less than 3.5% content in the film. Microscopic images of the films by scanning electron microscopy (SEM) and atomic force microscopy (AFM) showed formation of grains of approximately 20-40 nm in size on the film surfaces. The root-mean-square surface roughness from an AFM image was ${\sim}10{\AA}$. The interfacial layer of the $Ga_2O_3$/Si was measured to be ${\sim}35{\AA}$ thick by cross-sectional transmission electron microscopy (TEM). From the analysis of gaseous products of the CVD reaction by gas chromatography-mass spectrometry (GC-MS), an effort was made to explain the CVD mechanism.

Analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans to assure safety of imported meat (수입 식육의 안전성 확보를 위한 polychlorinated dibenzo-p-dioxins와 dibenzofurans 분석)

  • Kim, MeeKyung;Kim, Dong-Gyu;Kim, Sooyeon;Choi, Si-Weon;Kwon, Jin-Wook;Yun, Seon Jong;Song, Sung Ok;Chung, Gab Soo
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.39-48
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    • 2008
  • Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) are ubiquitous and can contaminate the food chain. A study monitoring PCDD/Fs in imported meat was conducted at the National Veterinary Research and Quarantine Service (NVRQS, Republic of Korea) in order to maintain food safety from the bioaccumulative PCDD/Fs. Seventeen PCDD/Fs with toxic equivalency factors (TEFs) established by World Health Organization (WHO, 1998) were analyzed in imported beef, pork, and chicken by high resolution gas chromatography/mass spectrometry (HR-GC/MS). Results of the monitoring for the last 5 years are presented. The levels of PCDD/Fs were similar to other studies except two unusually high concentrations in pork and beef. Excessive levels greater than the Korean provisional maximum residue limit of PCDD/Fs were found in a sample of pork imported from Chile and a sample of beef imported from U.S, and those products were rejected and returned. There was no obvious trend or differences with respect to time or origin of meat in this study.

Dietary Exposure to 3-Monochloropropane-1,2-diol from Sauces and Instant Fried Noodle (Ramyun) Seasoning (소스류 및 라면 스프에 의한 3-Monochloropropane-1,2-diol의 식이 노출)

  • Kim, Hyun-Jung;Chun, Hyang-Sook;Ha, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.306-310
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    • 2007
  • As a preliminary study for risk assessment of 3-monochloropropane-1,2-diol (3-MCPD) from processed food, the levels of 3-MCPD in commercial sauces and instant fried noodle (ramyun) seasoning were analyzed with gas chromatography/mass spectrometry. In August and September 2005, twenty-five samples of commercial sauces and twenty-five samples of instant fried noodle (ramyun) seasoning were collected from retail outlets and markets in Seoul, Korea. Six out of twenty-five sauces contained 3-MCPD and the highest concentration was 0.045 mg/kg. On the basis of per capita consumption of sauces and mean concentration of 3-MCPD, the estimated daily exposure to 3-MCPD from sauces was $0.094{\mu}g/person/day$. None of the twenty-five instant fried noodle (ramyun) seasoning samples was contained 3-MCPD. Therefore consumption of instant fried noodle (ramyun) seasoning was estimated not to contribute dietary exposure to 3-MCPD.

Characteristics and Antioxidative Activity of Volatile Compounds in Heated Garlic (Allium sativum)

  • Woo, Koan-Sik;Yoon, Hyang-Sik;Lee, Youn-Ri;Lee, Jun-Soo;Kim, Dae-Joong;Hong, Jin-Tae;Jeong, Heon-Sang
    • Food Science and Biotechnology
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    • v.16 no.5
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    • pp.822-827
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    • 2007
  • The aroma characteristics and antioxidative activity of volatile compounds in heat-treated garlic (Allium sativum L.) were evaluated. The garlic was heated to various temperatures (100, 110, 120, and $130^{\circ}C$) for different lengths of time (1, 2, and 3 hr). The volatile compounds of heated garlic were extracted by simultaneous steam distillation extraction (SDE). Aroma compound profiles were analyzed by gas chromatography/mass spectrometry (GC/MS) and antioxidative activity was measured by 2,2-diphenyl-2-picrylhydrazyl (DPPH) assay and 2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS) cation decolorization assay. The major aroma compounds were sulfur compounds such as dimethyl disulfide, 2-propen-1-ol, methyl-2-propenyl disulfide, dimethyl trisulfide, diallyl disulfide, methyl-2-propenyl trisulfide, and di-2-propenyl trisulfide. DPPH radical scavenging activity (EDA, %) and the ascorbic acid equivalent antioxidant activity (AEAC) of volatile compounds in heated garlic increased significantly with the increase of temperature and time (p<0.001). The EDA (%) and AEAC of raw garlic were 26.8%/10 mg garlic and 39.05 mg ascorbic acid equivalent per g sample. After heat treatment, the highest values were 40.50%/10 mg garlic for EDA (%) and 46.43 mg ascorbic acid equivalent per g sample for ABTS.

Flavor Compounds in Pine Mushroom Liquor Added with Pine Tree Chips (송절편을 첨가한 송이주의 향기 성분)

  • Yoon, Jeong-Ah;Shin, In-Ung;Park, Eun-Hee;Lee, Ha-Yeon;Kim, Myoung-Dong
    • Microbiology and Biotechnology Letters
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    • v.48 no.3
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    • pp.316-321
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    • 2020
  • Changes in flavor compounds in pine mushroom (Tricholoma matsutake) liquor added with pine tree chips were analyzed using gas chromatography/mass spectrometry. While three flavor compounds were detected in the control, fifteen were detected in the pine mushroom liquor added with pine tree chips. After eight-weeks of aging, the relative concentrations of β-fenchyl alcohol, 2-octanol, and methyl cinnamate, which are distinctive flavor characteristics of the pine mushroom, increased by 67.57%, 2.14%, and 0.94%, respectively, when pine tree chips were added (5%). Principal component analysis revealed that although flavor characteristics of the pine mushroom liquor were affected by the increased production of β-fenchyl alcohol due to the addition of pine tree chips, the aging time exerted a greater influence on flavor.

Investigating of Nitrosamines in Small tributary rivers, Sewage Tretment Plants and Drinking Water Treatment Plants (하천수 및 상하수도처리공정에서의 니트로사민류 조사)

  • Kim, Gyunga;Roh, Jaesoon;Bin, Jaehun;Kim, Changwon
    • Journal of Korean Society on Water Environment
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    • v.26 no.3
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    • pp.446-453
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    • 2010
  • This study was investigated nine nitrosamines in small tributary rivers, sewage treatment plants (STPs) and drinking water treatment plants. They are N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopyrrolidine (NPYR), N-nitrosodi-n-propylamine (NDPA), N-nitrosomorpholine (NMOR), N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPHA). The nine nitrosamines were analyzed by gas chromatography mass spectrometry (GC/MS) using solid phase extraction (SPE) with a coconut charcoal cartridge. Among the nine nitrosamines, NDMA, NMEA, NDEA, NDPA NDBA and NDPHA were detected in small tributary rivers and sewage tretment plants. In small tributary rivers, NDMA, NMEA, NDEA, NDPA, NDBA and NDPHA were obtained as ND~16.4 ng/L, ND~17.7 ng/L, ND~102.4 ng/L, ND~455.4 ng/L, ND~330.1 ng/L and ND~161.0 ng/L, respectively. Also NDMA, NMEA, NDEA, NDPA and NDBA were investigated ND~821.4 ng/L, 22.5~55.4 ng/L, 53.2~588.5 ng/L, ND~56.6 ng/L and ND~527.9 ng/L in STPs, respectively. In drinking water treatment plants, NMEA and NDEA concentration were increased to as high as 38.8 ng/L after ozonation process. However nitrosamines were decreased subsequent biological activated carbon (BAC) treatment process. It was supposed that nitrosamines were formed by $O_3$ oxidation and were removed by biodegradation of BAC.