• Title/Summary/Keyword: Mass Spectrometry (MS)

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Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.136-142
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    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

Risk Assessment of Heavy Metals Migrated from Plastic Food Utensils, Containers, and Packaging Distributed in Korea (국내 유통 식품용 플라스틱 기구 및 용기, 포장의 중금속 위해도 평가)

  • Kyung Youn, Lee;Hyung Soo, Kim;Dae Yong, Jang;Ye Ji, Koo;Seung Ha, Lee;Hye Bin, Yeo;Ji Su, Yoon;Kyung-Min, Lim;Jaeyun, Choi
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.28 no.3
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    • pp.175-182
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    • 2022
  • Heavy metals can be intentionally or unintentionally introduced into plastic food utensils, containers, and packaging (PFUCP) as additives or contaminants, which can be ingested with food by humans. Here, seven-heavy metals (lead, cadmium, nickel, chromium, antimony, copper, and manganese) with toxicity concerns were selected, and risk assessment was done by establishing their migration from 137 PFUCP products made of 16 materials distributed in Korea. Migration of heavy metals was examined by applying 4% acetic acid as a food simulant (70℃, 30 minutes) to the PFUCP products. Inductively coupled plasma mass spectrometry (ICP-MS) was employed for the analysis of migrated heavy metals, and the reliability of quantitative results was confirmed by checking linearity, LOD, LOQ, recovery, precision, and expanded uncertainty. As a result of monitoring, heavy metals were detected at a level of non-detection to 8.76 ± 11.87 ㎍/L and most of the heavy metals investigated were only detected at trace amounts of less than 1 ㎍/L on average. However, antimony migrated from PET products was significantly higher than other groups. Risk assessment revealed that all the heavy metals investigated were safe with a margin of exposure above 311. Collectively, we demonstrated that heavy metals migrated from PFUCP products distributed in Korea appear to be within the safe range.

The content and risk assessment of heavy metals in commercial herbal medicines (서울지역 유통한약재의 중금속 함량 및 위해성 평가)

  • Young Shin;Sang-Hun Park;Seung-Hye Han;So-Hyun Park;Ji-Hye Kim;Hyun-Jung Jang;Ae-Kyoung Kim;Ju-Seung Park
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.267-280
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    • 2023
  • This study investigated the contents of Pb, Cd, As, and Hg for 4333 samples with 2 09 types of herbal medicines distributed in Seoul area from 2019 to 2021, and evaluated risk assessment according to medicinal part used and origin. The contents of heavy metals were analyzed by inductively coupled plasma mass spectrometry (ICP-MS) and mercury analyzer. The average contents (mg/kg) of heavy metals by medicinal parts were 0.123 to 1.290 for Pb, 0.018 to 0.131 for Cd, 0.034 to 0.290 for As, and 0.003 to 0.015 for Hg. The contents of Pb were higher in Leaves and Whole Herbs (above-ground part) than underground part (Radix & Rhizoma) (ANOVA-test, p < 0.05). The contents of Cd were high in Leaves, Radix & Rhizoma, and Stems & Woods (ANOVA-test, p <0 .05), and exceeded regulatory limits in various types. Levels of Pb, Cd concentrations exceeding regulatory limits were observed in 8, 22 samples (8, 14 types). No sample exceeded regulatory limits of As and Hg. In the comparison between countries of origin, the contents of Cd, As, and Hg were high in imported herbal medicines (t-test, p < 0.05). As a result of the risk assessment, except for Thujae Orientalis Folium and Spirodelae Herba, the MOE values of Pb were all 1 or more, and most samples were safe. The Hazard Index (HI) for Cd, As, and Hg were evaluated to be less than 100 % even if the risk (%) of each heavy metal was added, and the risk from taking herbal medicines was evaluated to be safe.

Comparative Analysis of Ginsenoside Content in Processed Red Ginseng Foods Based on Food Type and Formulation (홍삼가공식품의 식품유형별 및 제형별 진세노사이드 함량 비교)

  • Yun-Jeong Yi;Min-Su Chang;In-Sook Lee;Hyun-Jeong Kim;Hyun-Jeong Jang;In-Sook Hwang
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.163-170
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    • 2024
  • Red ginseng is manufactured as a health-functional food and is also present in various food types and in different product forms. However, there is currently no standardized regulation of ginsenoside content in foods containing red ginseng. In the present study, we analyzed the ginsenoside content of 66 red ginseng-containing foods and 35 health-functional foods collected online and directly from the market. The ginsenoside content was assessed using liquid chromatography (LC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods. The ginsenoside content of the various food types ranged 0.0 (not detected)-71.567 mg per daily intake of foods containing red ginseng. Sugar-preserved foods had the highest ginsenoside content, followed by solid teas, liquid teas, and red ginseng beverages. For health-functional foods, the ginsenoside content ranged 3.4-58.5 mg per daily intake, with levels ranging 83-607% of the indicated amounts. All values met the established standards. Upon comparing red ginseng health-functional foods and red ginseng-containing foods, the average ginsenoside content was determined to be 18.21 and 8.79 mg, respectively, thus being nearly twice as high in health-functional foods. However, there was a minimal difference between the ginsenoside content of red and black ginseng, with values of 11.84 and 12.63 mg, respectively. These findings provide insights on the variations in ginsenoside content of red and black ginseng in various food forms. This information is expected to be valuable for future regulations and consumer choice of products containing red ginseng.

Radiosynthesis of $[^{11}C]6-OH-BTA-1$ in Different Media and Confirmation of Reaction By-products. ($[^{11}C]6-OH-BTA-1$ 조제 시 생성되는 부산물 규명과 반응용매에 따른 표지 효율 비교)

  • Lee, Hak-Jeong;Jeong, Jae-Min;Lee, Yun-Sang;Kim, Hyung-Woo;Lee, Eun-Kyoung;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.3
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    • pp.241-246
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    • 2007
  • Purpose: $[^{11}C]6-OH-BTA-1$ ([N-methyl-$^{11}C$]2-(4'-methylaminophenyl)-6-hydroxybenzothiazole, 1), a -amyloid imaging agent for the diagnosis of Alzheimer's disease in PET, can be labeled with higher yield by a simple loop method. During the synthesis of $[^{11}C]1$, we found the formation of by-products in various solvents, e.g., methylethylketone (MEK), cyclohexanone (CHO), diethylketone (DEK), and dimethylformamide (DMF). Materials and Methods: In Automated radiosynthesis module, 1 mg of 4-aminophenyl-6-hydroxybenzothiazole (4) in 100 l of each solvent was reacted with $[^{11}C]methyl$ triflate in HPLC loop at room temperature (RT). The reaction mixture was separated by semi-preparative HPLC. Aliquots eluted at 14.4, 16.3 and 17.6 min were collected and analyzed by analytical HPLC and LC/MS spectrometer. Results: The labeling efficiencies of $[^{11}C]1$ were $86.0{\pm}5.5%$, $59.7{\pm}2.4%$, $29.9{\pm}1.8%$, and $7.6{\pm}0.5%$ in MEK, CHO, DEK and DMF, respectively. The LC/MS spectra of three products eluted at 14.4, 16.3 and 17.6 mins showed m/z peaks at 257.3 (M+1), 257.3 (M+1) and 271.3 (M+1), respectively, indicating their structures as 1, 2-(4'-aminophenyl)-6-methoxybenzothiazole (2) and by-product (3), respectively. Ratios of labeling efficiencies for the three products $([^{11}C]1:[^{11}C]2:[^{11}C]3)$ were $86.0{\pm}5.5%:5.0{\pm}3.4%:1.5{\pm}1.3%$ in MEK, $59.7{\pm}2.4%:4.7{\pm}3.2%:1.3{\pm}0.5%$ in CHO, $9.9{\pm}1.8%:2.0{\pm}0.7%:0.3{\pm}0.1%$ in DEK and $7.6{\pm}0.5%:0.0%:0.0%$ in DMF, respectively. Conclusion: The labeling efficiency of $[^{11}C]1$ was the highest when MEK was used as a reaction solvent. As results of mass spectrometry, 1 and 2 were conformed. 3 was presumed.

Monitoring Heavy Metals in Meat and Meat Products (식육 및 그 가공품의 중금속 모니터링)

  • Hwang, Tae-Ik;Ahn, Tae-Hyun;Kim, Eun-Jung;Lee, Jung-Ah;Kang, Myoung-Hee;Jang, Young-Mi;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.525-531
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    • 2011
  • This study was conducted to examine the contents of lead (Pb), cadmium (Cd), arsenic (As), and mercury (Hg) in meat and meat products in Korea. The contents of Pb, Cd, As, and Hg in 466 samples of beef, pork, chicken, duck, ham, and sausage were measured using inductively coupled plasma mass spectrometry or a mercury analyzer. Wet ashing and microwave method were compared, and the recovery and reproducibility of the microwave method were better than those of wet ashing for meat and meat products. The recovery of the microwave method was 98.1% for Pb, 104.6% for Cd, and 103.4% for As, respectively. The best result was obtained through digestion using an acid mixture ($HNO_3$/$H_2O_2$, 6:2). Hg content was measured using a mercury analyzer. As a result, the contents of Hg and Cd in samples were lower than those of Pb and As. The average contents of Pb were 0.009 mg/kg in beef, 0.010 mg/kg in pork, 0.006 mg/kg in chicken, 0.007 mg/kg in duck, 0.005 mg/kg in ham, and 0.009 mg/kg in sausage. The average Cd contents were 0.0004 mg/kg in beef, 0.0004 mg/kg in pork, 0.0005 mg/kg in chicken, 0.0012 mg/kg in duck, 0.0015 mg/kg in ham, and 0.0019 mg/kg in sausage. The average As contents were 0.016 mg/kg in beef, 0.004 mg/kg in pork, 0.021 mg/kg in chicken, 0.010 mg/kg in duck, 0.014 mg/kg in ham, and 0.018 mg/kg in sausage. The average Hg contents were 0.713 ${\mu}g/kg$ in beef, 0.902 ${\mu}g/kg$ in pork, 0.710 ${\mu}g/kg$ in chicken, 0.796 ${\mu}g/kg$ in duck, 1.141 ${\mu}g/kg$ in ham, and 1.052 ${\mu}g/kg$ in sausage. Based on the results of the National Health and Nutrition Survey 2005, the levels of dietary exposure to heavy metal contaminants in meat and meat products were compared with the provisional tolerable weekly intake(PTWI) established by the Joint FAO/WHO Expert Committee on Food Additives. The average dietary exposure of the general population from meat and meat products was 0.03-0.2% of PTWI for Pb, Cd, As, and Hg, which indicates a safe level for public health at present.

Correlation between Steroid Hormone Metabolites and Leiomyomas of Uterus (자궁근종과 성호르몬 대사물과의 연관성)

  • Bai, Sang-Wook;Jung, Byung-Hwa;Chung, Bong-Chul;Jeon, Jin-Dong;Lee, Hyun-Jung;Kwon, Han-Sung;Chung, Kyung-Ah;Kim, Sei-Kwang;Park, Ki-Hyun
    • Clinical and Experimental Reproductive Medicine
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    • v.28 no.4
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    • pp.279-286
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    • 2001
  • Objective: To elucidate 1) whether there are any differences in the urine concentrations of steroid hormone metabolites between patients with leiomyoma and normal controls 2) the correlation between urinary profiles of steroid hormones and leiomyomas of the uterus according to their type, location, volume, and weight. Materials of Methods : The study population consisted of 37 premenopausal patients with uterine leiomyoma and the control group consisted of 25 premenopausal normal volunteer women without uterine leiomyoma. Confirmation of the existence of uterine leiomyoma was done by ultrasonography and histopathological examination after surgery. The volume of the leiomyoma was estimated by trans-abdominal and/or trans-vaginal ultrasonography. The Leiomyomas were divided into 3 types (subserosal, intramural and submucosal). Seventeen patients had subserosal type of leiomyoma, 10 with the intramural type and 10 with the submucosal type. The locations of the leiomyoma were also divided into 3 groups (fundus, body and isthmus). Seventeen patients showed a fundus location, 10 in body, and 10 in isthmus. We compared urinary profiles of the endogenous steroids between patients with leiomyomas and normal controls, and also investigated the relationship between urinary profiles of the endogenous steroids and leiomyomas according to their type, location, volume and weight by using highly sensitive Gas Chromatography-Mass Spectrometry (GC-MS) system. Results: The mean ages of the patients with leiomyomas and the control group were $43.1{\pm}5.6$ and $40.6{\pm}7.2$ years, the weights were $63.4{\pm}7.3$ and $59.4{\pm}8.1\;kg$, and their heights were $155.4{\pm}4.8$ and $159.3{\pm}4.8\;cm$ respectively. Seventeen patients had subserosal, 10 had intramural, and 10 had submucosal leiomyomas. There were 17 patients with leiomyoma located in fundus, 10 in body and 10 in isthmus. $17{\beta}$-estradiol, 5-AT, 11-keto ET, $11{\beta}$-hydroxy An, $11{\beta}$-hydroxy Et, THS, THA, THE, a-cortolone, a-cortol, $\beta$-cortol, $11{\beta}$-OH Et/$11{\beta}$-OH An and E2/E1 were significantly increased in patients with leiomyoma than in the control group. $17{\beta}$-estradiol was significantly increased in the intramural and the submucosal types than in the subserosal type. There was no significant difference in the concentrations of urinary steroids according to the locations of leiomyomas. There was no significant relationship between the concentration of urinary steroids and the volume of the leiomyomas. $17{\beta}$-estradiol significantly decreased as the weight of uterus increased (r=-0.322, p=0.04). Conclusion: The concentrations of steroid hormone metabolites were generally increased in patients with leiomyoma but were not significantly related to the volume and weight of the leiomyomas. Our study suggests that steroid hormones may be involved in the initiation of leiomyomas but may not be involved in their progression. In addition, the concentrations of steroid hormone metabolites are not related to the leiomyoma type and location.

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Estimated Daily Intake of Aluminum from Platycodon grandiflorum A. De Candolle (도라지(Platycodon grandiflorum A. De Candolle) 섭취에 따른 알루미늄의 노출량 평가)

  • Kim, Sung-Dan;Ham, Hee-Jin;Jung, Ji-Hun;Lee, Eun-Soon;Lee, Hyun-Kyung;Kim, Hee-Sun;Lee, Jib-Ho;Yu, In-Sil;Jung, Kweon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.8
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    • pp.1138-1146
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    • 2016
  • This study was performed to estimate daily intakes of aluminum from Platycodon grandiflorum A. De Candolle and evaluate their potential health risks for Koreans. Estimated daily intake of aluminum was calculated, whereas the actual level of aluminum in Platycodon grandiflorum A. De Candolle was analyzed using inductively coupled plasma mass spectrometry. Food consumption amount was drawn from Korea National Health and Nutrition Examination Survey (KNHANES VI-1). In analysed samples, aluminum values ranged from 0.54~564.38 mg/kg in peeled Platycodon grandiflorum A. De Candolle samples (n=53) and from 0.72~28.05 mg/kg in unpeeled ones (n=40). Statistically significant difference (P<0.001) was detected according to the type of skin. To estimate the dietary intake of Platycodon grandiflorum A. De Candolle, a total of 7,242 respondents (scenario I) were compared to 227 Platycodon grandiflorum A. De Candolle consumption subjects (scenario II). Estimated daily intake of aluminum was calculated based on point estimates. Level of safety for aluminum was evaluated by comparison with Provisional Tolerable Weekly Intake (PTWI), 1 mg/kg bw, set by the Joint FAO/WHO Expert Committee on Food Additives. For scenario I, mean estimated daily intake of aluminum was 0.001 mg/kg bw/d. For scenario II, mean estimated daily intake of aluminum was 0.033 mg/kg bw/d, and 95th percentile estimated daily intake was 0.610 mg/kg bw/d. For scenario II, aluminum from Platycodon grandiflorum A. De Candolle had a mean weekly intake that was the 23.1% of PTWI.

Aroma Characteristics of Byeolmijang with Optional Ingredients (부재료 첨가에 따른 별미장의 향기특성)

  • Woo, Koan-Sik;Han, Seo-Young;Yoon, Hyang-Sik;Lee, Jun-Soo;Jeong, Heon-Sang;Kim, Haeng-Ran
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.6
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    • pp.738-746
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    • 2006
  • Aroma compounds in four different Byeolmijang made from optional ingredient addition were extracted by SDE (simultaneous steam distillation extraction) and analyzed with GC (gas chromatography) and GC/MS (mass-spectrometry). The major aroma compounds in the four different Byeolmijang during aging were 1-octene-3-ol, hexanal, benzeneacetaldehyde, benzaldehyde, fufural, pyrazine, furan and phenol type compounds. Generally, benzeneacetaldehyde, benzaldehyde, fufural and phenol type compounds were increased during aging. On the other hand, 1-octen-3-ol, hexanal and furan were decreased during aging. Furfural, 2-furanmathanol and benzeneacetaldehyde in Sanghwangjang, 3-methyl-1-butanol, phenol and 1H-indole in Mujang, hexanal, 1-octen-3-ol and 2,4-decadienal in Bizijang and hexanal, tetramethylpyrazine and 2-methoxy-4-vinylphenol in Jigeumjang were identified as major aroma compounds, respectively. Generally, the major aroma compound in four different Byeolmijang with optional ingredient was similar with control and pyrazine, furan and phenol type compounds were decreased to addition with optional ingredient. The major aroma compound in Sanghwangjang with optional ingredient (onion) were 1-hexanol and 2,5-dimethylthiophene and the major aroma compounds were 1,2,4-trithiolane and 2-buthyl-2-octenal in Mujang with optional ingredient (Letinus edodes). Furfural, benzaldehyde, benzeneacetaldehyde, 1,2,4-trithiolane and lenthionine were detected in Bizijang due to the addition of powdered Letinus edodes. Linaool and ${\beta}-lonone$ were detected in Jigeumjang due to the addition of powdered red pepper.

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.