• Title/Summary/Keyword: Liquid Chromatography-tandem Mass Spectrometry

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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.

Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Method Development for Determination of Multi-Mycotoxins in Chicken Liver and Kidney Tissues by LC-MS/MS (LC-MS/MS를 이용한 닭 간과 신장 중 곰팡이 독소 6종 동시분석법 개발)

  • Kim, Soohee;Kim, Kwang-Nam;Kim, Hyobi;Song, Jae-Young;Park, Sung-Won
    • Korean Journal of Poultry Science
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    • v.43 no.2
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    • pp.111-118
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    • 2016
  • Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

Monitoring and Risk Assessment of Pesticide Residues Farmers' Market Produce in Northern Gyeonggi-do (경기 북부 내 직거래 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Lim, Jeong-Hwa;Park, Po-Hyun;Lim, Bu-Geon;Ryu, Kyong-Shin;Kang, Min-Seong;Song, Seo-Hyeon;Kang, Nam-Hee;Yoo, Na-Young;Kim, Jeong-Eun;Kang, Choong-Won;Kim, Youn-Ho;Seo, Jeong-Hwa;Choi, Ok-Kyung;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.35 no.3
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    • pp.243-251
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    • 2020
  • In this study, we investigated pesticide residues in 207 agricultural products distributed by direct trade in the northern area of Gyeonggi Province. A total of 94 general agricultural products and 113 eco-friendly agricultural products collected from local grocers and cooperative stores were analyzed by multiresidue method for 263 pesticides using GC (gas chromatography)/ECD (electron capture detector), GC/NPD (nitrogen phosphorus detector), GC-MS/MS (tandem mass spectrometry), LC (liquid chromatography)/PDA (photodiode array detector), LC/FLD (fluorescence detector), LC-MS/MS. All samples showing pesticide residues were general agricultural products collected from local food stores. The pesticide residue levels of 14 samples (6.8%) were below the maximum residue limits (MRLs) and one of them (0.5%) exceeded the MRLs. Sixteen pesticides were detected from samples of the following produce items: spinach, young cabbage, perilla leaves, mallow, cucumber, chives and water dropwort. The safety of the detected pesticides was assessed by monitoring the daily intake estimate (EDI) and the daily intake allowance (ADI) based on the amount of pesticides detected. The ADI percentage range (the ratio of EDI to ADI) was 0.0134-61.6259% and there was no health risk connected with consuming agricultural products in which pesticide residues were detected.

Analysis of ethyl glucuronide (EtG) in Hair for the diagnosis of chronic alcohol abuse of Korean (한국인의 만성 알코올 중독 진단을 위한 모발에서 Ethyl Glucuronide (EtG) 분석법 연구)

  • Gong, Bokyoung;Jo, Young-Hoon;Ju, Soyeong;Min, Ji-Sook;Kwon, Mia
    • Analytical Science and Technology
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    • v.33 no.3
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    • pp.151-158
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    • 2020
  • Alcohol, which can easily be obtained in the same way as ordinary beverages, is harmful enough to cause death due to excessive drinking and chronic alcohol intake, so it is important to maintain a proper amount of drinking and healthy drinking habits. In addition, the incidence of behavioral disturbances and impaired judgments that can be caused by chronic alcohol drinking of more than adequate amounts of alcohol is also significant. Accordingly it is very useful for forensic science to check whether the person involved is drunken or is alcoholism state in various accidents. Currently, in Korea, alcohol consumption is determined by detecting the level of alcohol or alcohol metabolism 'ethyl glucuronide (EtG)' in blood or urine samples. However, analysis of alcohol or EtG in blood or urine can only provide information about the current state of alcohol consumption because of a narrow window of detection time. Therefore, it is important to analyze the EtG as a long-term direct alcohol metabolite bio-marker in human hair and to investigate relationship between alcohol consumption and EtG concentration for the evaluation of chronic ethanol consumption. In this study, we established an analytical method for the detection of EtG in Korean hair efficiently and validated selectivity, linearity, limits of detection (LOD), limits of quantification (LOQ), matrix effect, recovery, process efficiency, accuracy and precision using liquid chromatography tandem mass spectrometry (LC-MS/MS). In addition, the assay performance was evaluated in Korean social drinker's hair and the postmortem hair of a chronic alcoholism. The results of this study can be useful in monitoring the alcohol abuse of Korean in clinical cases and legal procedures related to custody and provide a useful tool to evaluate postmortem diagnosis of alcoholic ketoacidosis in forensics.

Bioconcentration Factor(BCF) of Perchlorate from Agricultural Products and Soils (농산물과 토양에 대한 퍼클로레이트 함량 평가 및 생물농축계수 산출)

  • Kim, Ji-Young;Kim, Min-Ji;Lee, Jeong-Mi;Kim, Doo-Ho;Park, Ki-Moon;Kim, Won-Il
    • Korean Journal of Environmental Agriculture
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    • v.32 no.3
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    • pp.224-230
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    • 2013
  • BACKGROUND: Perchlorate(${ClO_4}^-$) is an anion that is extremely water-soluble and environmentally stable. It mostly exists in the form of sodium perchlorate, ammonium perchlorate and potassium perchlorate which are used in rocket fuels, propellants, ignitable sources, air bag inflation systems and explosives. Perchlorate can be taken into the thyroid glands and interfere with iodide uptake. The determination of perchlorate in agricultural products is important due to its potential health impact on humans. The objective of this study was to determine the perchlorate concentrations in the samples of various agricultural products and soils. METHODS AND RESULTS: In this study, samples of cereal(Rice, Barley, Corn, Bean), vegetable(Spinach, Lettuce, Sesame, Chives, Chili, Pumpkin, Tomato), fruit(Apple, Pear, Tangerine, Grape) were analyzed for perchlorate contents. Perchlorate concentrations were analyzed by liquid chromatography-tandem mass spectrometry. The results showed that agricultural products respectively contained perchlorate concentrations in the range of : cereals N.D.~$7.46{\mu}g/kg$, vegetables $0.52{\sim}23.06{\mu}g/kg$, fruits $0.19{\sim}2.66{\mu}g/kg$. Bioconcentration factor was in the order of : vegetables > cereals > fruits. Bioconcentration factor was highest follwed by Sesame 37.88, Corn 21.51, Spinach 10.57, Tangerine 4.39, Chives 2.89 and Lettuce 1.90. The recoveries of perchlorate from spiked agricultural products and soils ranged from 87.72~111.26% and 102.09~111.23%. CONCLUSION(S): The health risk assessment results obtained in this study are lower than the RfD(Reference Dose, 0.0007 mg/kg/body weight/day) value as suggested by the Integrated Risk Information System(US IRIS). Our results indicate that, people currently exposed to perchlorate from agricultural products consumption are considered as safe.

Characterization of Antibacterial Compounds from Bacillus polyfermenticus CJ6 and Its Growth Inhibition Effect on Food-Borne Pathogens (Bacillus polyfermenticus CJ6가 생산하는 항세균 물질의 특성 및 병원성 식중독 미생물의 성장 억제 효과)

  • Jung, Ji-Hye;Chang, Hae-Choon
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.6
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    • pp.903-911
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    • 2011
  • In this study, Bacillus polyfermenticus CJ6 harboring antibacterial activity was isolated from meju. The antibacterial activity of Bacillus polyfermenticus CJ6 was stable in the pH range of 3.0~9.0, but it disappeared after culture at $70^{\circ}C$ for 24 hr. Antibacterial activity was inactivated by proteinase K, protease, and ${\alpha}$-chymotrypsin, indicating its proteinaceous nature. The growth inhibitory effects of B. polyfermenticus CJ6 culture on food-borne pathogens such as Staphylococcus aureus, Salmonella Typhi, Listeria monocytogenes, and Escherichia coli O157:H7 were examined in this study. Approximately 6~6.2 log CFU/mL of each pathogen was co-cultured with B. polyfermenticus CJ6 in a 50 mL culture volume for 24 hr. Growth of S. aureus and L. monocytogenes was completely inhibited after 3 hr of incubation. Growth of S. Typhi and E. coli O157:H7 was also completely inhibited after 6 hr of incubation. The antibacterial compounds from B. polyfermenticus CJ6 were purified by solid phase extraction (C18 Sep-pak cartridge), recycling preparative HPLC, and analytical HPLC. Ultra-high performance liquid chromatography and electrospray ionization tandem mass spectrometry analysis were used to identify the purified antibacterial compounds, which were confirmed to be five peptides (757.4153 Da, 750.3444 Da, 1024.5282 Da, 1123.6083 Da, and 1617.8170 Da).

Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS (HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구)

  • Kim, Jong-Hwa;Moon, Sun-Ea;Kim, Ki-Yu;Jung, You-Jung;Lee, Chang-Hee;Ku, Eun-Jung;Yoon, Mi-Hye;Lee, Jong-Bok
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.94-98
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    • 2016
  • This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.

한국인 좌심실 비대증 환자들에서 파브리병 선별검사의 의의

  • Park, Hyeong-Du;Jo, Seong-Yun;Lee, Su-Yeon;Jeon, Eun-Seok;Park, Seung-U;Lee, Sang-Hun;Lee, Sang-Cheol;Choe, Jin-O;Park, Seong-Ji;Jang, Seong-A;Kim, Hyeong-Gwan;Gi, Chang-Seok;Kim, Jong-Won;Jin, Dong-Gyu
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.14 no.2
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    • pp.135-141
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    • 2014
  • Objectives: Fabry disease (FD) is a lysosomal storage disease caused by the inappropriate accumulation of globotriaosylceramide (Gb3) in tissues due to a deficiency in the enzyme ${\alpha}$-galactosidase A. Hypertrophic cardiomyopathy is one of the chronic complications of FD. We tried to evaluate the prevalence of Fabry disease in the Korean patients with left ventricular hypertrophy (LVH). Methods: A total of 257 patients with LVH were recruited and they were 172 males (mean 56 years, range 30-81 years) and 84 females (mean 66 years, range 45-85 years). Urinary Gb3 was used to screen FD by high performance liquid chromatography-tandem mass spectrometry. Confirmatory tests were done by alpha-galactosidaseA activity using fluorometric assay and by GLA mutation analysis using sequencing. Results: Four patients were screening positive by urinary Gb3 analysis (cutoff, 25 ug/mmol creatinine). But, one female patient was diagnosed with FD confirmed by enzyme analysis in leukocytes as well as by genetic analysis (1/257 patients, 0.4%). She showed 54.3 ug/mmoL creatinine of Gb3 and 15.5 nmole/hr/mg protein (reference range, $55.2{\pm}12.7nmole/hr/mg$ protein) of alphagalactosidase A activity. And she had a heterozygous GLA mutation of c.796G>A (p.D266N). Her daughter was found to be a carrier for FD confirmed by GLA mutation analysis. Asymptomatic carrier showed 25.5ug/mmol creatinine of Gb3 and 42.5 nmole/hr/mg protein (reference range, $55.2{\pm}12.7nmole/hr/mg$ protein) of alpha-galactosidase A activity. Conclusions: The prevalence of FD in Koran patients with LVH was detected as 0.4%. Although the prevalence seems to be low, screening studies are of great importance for detecting hidden cases as well as for identifying other effected family members.

Evaluation of Residual Pesticides in Commercial Agricultural Products Using LC-MS/MS in Korea (LC-MS/MS를 이용한 한국에서 유통되는 농산물의 잔류 농약 평가)

  • Lee, Hwa-Mi;Hu, Soo Jung;Lee, Hyun-Sook;Park, Seung Young;Kim, Nam-Sun;Shin, Yong Woo;Choi, Keun Hwa;Kim, Sung Il;Nam, Seul Yi;Cho, Dae Hyun
    • Korean Journal of Food Science and Technology
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    • v.45 no.4
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    • pp.391-402
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    • 2013
  • Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.