• Title/Summary/Keyword: tandem mass spectrometry #4

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Monitoring of Residual Pesticides and Exposure Assessment of Olive Oil Products Sold on the Market (올리브유의 잔류농약 모니터링 및 노출량 조사)

  • Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.4
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    • pp.211-216
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    • 2023
  • A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

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.

Determination of plasma C16-C24 globotriaosylceramide (Gb3) isoforms by tandem mass spectrometry for diagnosis of Fabry disease (패브리병(Fabry) 진단을 위한 혈장 중 Globotriaosylceramide (Gb3)의 탠덤매스 분석법 개발과 임상 응용)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Yoo, Han-Wook;Choi, Jin-Ho;Lee, Dong-Hwan;Zhang, Kate;Keutzer, Joan
    • Journal of Genetic Medicine
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    • v.4 no.1
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    • pp.45-52
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    • 2007
  • Purpose : A simple, rapid, and highly sensitive analytical method for Gb3 in plasma was developed without labor-ex tensive pre-treatment by electrospray ionization MS/ MS (ESI-MS/MS). Measurement of globotriaosy lceramide (Gb3, ceramide trihex oside) in plasma has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. Methods : Only simple 50-fold dilution of plasma is necessary for the extraction and isolation of Gb3 in plasma. Gb3 in diluted plasma was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Results : Eight isoforms of Gb3 were completely resolved from plasma matrix. C16:0 Gb3 occupied 50% of total Gb3 as a major component in plasma. Linear relationship for Gb3 isoforms w as found in the range of 0.001-1.0 ${\mu}g$/mL. The limit of detection (S/N=3) was 0.001 ${\mu}g$/mL and limit of quantification was 0.01 ${\mu}g$/mL for C16:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9678 to 0.9982. Conclusion : This quantitative method developed could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

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Monitoring of Pesticide Residues and Heavy Metals in Fermented Liquor in Ulsan (울산지역 유통 발효주의 잔류농약 및 중금속 실태조사)

  • Hee-Jung Kim;Kyoung-Jin Kim;Min-Kyung Kim;Geum-Bi Kim;Su-Hee Kim;Young-Kyung Jo;Ju-Eun Park;So-Yeon Jeong;Won-Dug Seo;Young-Sun Choi
    • Journal of Food Hygiene and Safety
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    • v.39 no.3
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    • pp.250-259
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    • 2024
  • In this study, we investigated in pesticide residues and heavy metals in fermented liquor products (wine, beer, makgeolli). Targeted analysis of 400 pesticide residues in the sample was performed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method, followed by gas chromatography-tandem mass spectrometry (MS/MS) and LC-MS/MS. The contents of heavy metals (Pb, Cd) were determined by ICP-MS using the microwave method. The mercury was measured using a mercury analyzer. From the analysis of 150 cases, 102 (68.0%) cases of fermented liquor were detected, and 35 pesticide residues (including metalaxyl, mandipropamid, azoxystrobin, and fenhexamid) were detected among the 400 pesticide residues tested. Pb, Cd, and Hg were tested in 150 samples. Lead was detected in 73 samples (48.7%), cadmium in 9 samples (6.0%), and mercury in 36 samples (24.0%). Exposure assessment was conducted to determine the safety of the detected pesticide residues and heavy metals. According to this assessment, the pesticide residues and heavy metals showed very low %ADI values (less than 1%).

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.