• Title/Summary/Keyword: Drug safety data

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Establishment of a library of fragments for the rapid and reliable determination of anabolic steroids by liquid chromatography-quadrupole time of flight-mass spectrometry

  • Do, Jung-Ah;Noh, Eunyoung;Yoon, Soon-Byung;Choi, Hojune;Baek, Sun-Young;Park, Sung-Kwan;Lee, Sang-Gyeong
    • Analytical Science and Technology
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    • v.30 no.1
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    • pp.10-19
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    • 2017
  • Anabolic steroids have similar structures to testosterone, both of which promote the growth of muscle mass and increase strength. However, the side effects of anabolic steroid use may lead to heart attacks or strokes. Additionally, the excessive use of steroids inhibits the production of the sex hormones in the body via a negative feedback loop, which results in testicular atrophy in males and amenorrhea in females. Currently, the method of choice used to test for the presence of anabolic steroids is GC-MS. However, GC-MS methods require chemical derivatization of the steroid sample to ensure compatibility with the analytical method; therefore, analysis of many different samples is difficult and time consuming. Unlike GC-MS, the liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) method is suitable for many samples. Twenty-two different anabolic steroids were analyzed by LC-Q-TOF-MS with various collision energies (CE). Accurate mass spectral data were obtained using a Q-TOF-MS equipped with an electro-spray ionization source and operated in the positive MS/MS mode for several classes of steroids that are often the targets of testing. Based on the collected data, fragmentation pathways were carefully elucidated. The high selectivity and sensitivity of the LC-Q-TOF-MS instrument combined with these fragmentation pathways offers a new approach for the rapid and accurate screening of anabolic steroids. The obtained data from the 22 different anabolic steroids will be shared with the scientific community in order to establish a library to aid in the screening of illegal anabolic steroids.

Study on the Antioxidant Activity in the Various Vegetables (채소류의 항산화 효과 비교 연구)

  • Suh, Junghyuck;Paek, Ock Jin;Kang, YoungWoon;Ahn, Ji Eun;Yun, Jisuk;Oh, Keum-Soon;An, Yeong-Soon;Park, Sun-Hee;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.28 no.4
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    • pp.337-341
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    • 2013
  • After it was known that an antioxidant function was associated with a reducing risk of cancer and cardiovascular disease, a large number of plant have been investigated for their antioxidant activity. However, lacking of the extensive antioxidant data in vegetables, a few natural antioxidant was used in the food industry. Therefore, this study was carried out to provide some scientific antioxidant activity data in the various vegetables. The samples (n = 275) including 24 kinds of vegetables were examined for antioxidant activity. Total Phenol Contents (TPCs) were measured colorimetric determination method using the Folin-Ciocalteu reagent by gallic acid as the control group. DPPH radical scavenging activity were also investigated using calculation of $IC_{50}$(concentration of extracted needed to inhibit 50% of the DPPH radical). The contents of TPCs were $0.32{\sim}49.26{\mu}g/kg$ and DPPH radical scavenging activity ($CI_{50}$) was 0.0~2.43 mg/mL in vegetables. The best antioxidant effect was shown in Garlic for both antioxidant assay methods.

Screening and detection of methylisothiazolinone and chloromethylisothiazolinone in cosmetics by UPLC-MS/MS

  • Lee, Ji Hyun;Paek, Ji Hyun;Park, Han Na;Park, Seongsoo;Kang, Hoil
    • Analytical Science and Technology
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    • v.33 no.3
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    • pp.125-133
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    • 2020
  • Methylisothiazolinone (MIT) and chloromethylisothiazolinone (CMIT) cause allergic contact dermatitis and are banned cosmetics ingredients, except in rinse-off products. However, their presence has been detected in cosmetics. We report a UPLC-tandem MS/MS screening method for their simultaneous determination in cosmetics. To facilitate extraction from various matrices, pretreatment methods were developed for each sample type. The method was optimized through a series of assessments, including specificity, LOD, LOQ, linearity, recovery, stability, precision, and accuracy. The LODs and LOQs for MIT ranged from 0.054 and 0.163 ㎍ mL-1 whereas those for CMIT ranged from 0.040 and 0.119 ㎍ mL-1. The linear correlation coefficients (r2) were higher than 0.999. Relative standard deviations (RSDs) for both intra- and inter-day measurements ranged from 0.3 ~ 13.6 %. Recoveries at three different concentrations were within 87.9 ~ 118.9 %. The RSD for stability measurements of spiked samples was within 7 %. These results confirm the suitability of the developed method for the simultaneous quantitation of MIT and CMIT in cosmetics. Samples of 320 color cosmetics, including eyeshadows, solid lipsticks, liquid lipsticks, and nail polishes were analyzed using the developed method, and two of them were found to contain both MIT and CMIT and one of them was found to contain only MIT. This data and the method will aid the regulation of ingredients used in cosmetics.

Development of Simultaneous Analytical Method for Streptomycin and Dihydrostreptomycin Detection in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Streptomycin 및 Dihydrostreptomycin 동시시험법 개발)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Park, Shin-Min;Cho, Sung Min;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.1
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    • pp.13-21
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    • 2019
  • A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

Genetic Characteristics of Extended-Spectrum Beta-Lactamase-Producing Salmonella Isolated from Retail Meats in South Korea

  • Haiseong Kang;Hansol Kim;Hyochin Kim;Ji Hye Jeon;Seokhwan Kim;Yongchjun Park;Soon Han Kim
    • Journal of Microbiology and Biotechnology
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    • v.34 no.5
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    • pp.1101-1108
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    • 2024
  • Earlier studies have validated the isolation of extended-spectrum beta-lactamase-producing Salmonella (ESBL-Sal) strains from food. While poultry is recognized as a reservoir for Salmonella contamination, pertinent data regarding ESBL-Sal remains limited. Consequently, the Ministry of Food and Drug Safety has isolated Salmonella spp. from retail meat and evaluated their antibiotic susceptibility and genetic characteristics via whole-genome sequencing. To further elucidate these aspects, this study investigates the prevalence, antibiotic resistance profiles, genomic characteristics, and homology of ESBL-Sal spp. obtained from livestock-derived products in South Korean retail outlets. A total of 653 Salmonella spp. were isolated from 1,876 meat samples, including 509 beef, 503 pork, 555 chicken, and 309 duck samples. The prevalence rates of Salmonella were 0.0%, 1.4%, 17.5%, and 28.2% in the beef, pork, chicken, and duck samples, respectively. ESBL-Sal was exclusively identified in poultry meat, with a prevalence of 1.4% in the chicken samples (8/555) and 0.3% in the duck samples (1/309). All ESBL-Sal strains carried the blaCTX-M-1 gene and exhibited resistance to ampicillin, ceftiofur, ceftazidime, nalidixic acid, and tetracycline. Eight ESBL-Sal isolates were identified as S. Enteritidis with sequence type (ST) 11. The major plasmid replicons of the Enteritidis-ST11 strains were IncFIB(S) and IncFII(S), carrying antimicrobial resistance genes (β-lactam, tetracycline, and aminoglycoside) and 166 virulence factor genes. The results of this study provide valuable insights for the surveillance and monitoring of ESBL-Sal in South Korean food chain.

Development of Analytical Method for Kasugamycin in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Kasugamycin 시험법 개발)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.235-241
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    • 2019
  • An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

Identification and evaluation of fragmentation pathways of PDE-5 inhibitor analogues using LC-QTOF-MS (LC-QTOF-MS를 이용한 발기부전치료제 유사물질의 fragmentation pathway 분석)

  • Do, Jung-Ah;Noh, Eunyoung;Yoon, Soon-Byung;Park, Hyoung-Joon;Cho, Sooyeul;Park, Sung-Kwan;Yoon, Chang-Yong
    • Analytical Science and Technology
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    • v.28 no.4
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    • pp.278-287
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    • 2015
  • Phosphodiesterase type 5 inhibitors (PDE-5 inhibitors) are used in the treatment of erectile dysfunction. In recent years, a number of reports have been conducted on dietary supplements contaminated with PDE-5 analogues. In this study, 58 analogues of PDE-5 inhibitors were sorted into five groups: tadalafil, sildenafil, hongdenafil, vardenafil, and other analogues. These analogues were then evaluated using a liquid chromatography-quadrupole-time of flight mass spectrometry (LC-QTOF-MS) electrospray ionization mass method. Each compound has a unique fragmentation ion, which can be easily analyzed qualitatively. The fragmentation pathways of the analogues were elucidated based on the QTOF-MS and MS/MS data. Common ions were confirmed for each group by analyzing the structural characteristics and fragmentation pathways. Specifically, common ions were observed at m/z 169.08 and 135.04 (tadalafil analogues), m/z 311.15 and 283.12 (sildenafil analogues and hongdenafil analogues), and m/z 312.16 and 151.09 (vardenafil analogues). The advantage of this method is that the structure of unknown components can be determined by interpreting the product ions. Hence, the developed method can be used for the identification of unknown compounds. Fragmentation pathways may also aid in the detection and identification of PDE-5 inhibitor analogues.

Dependence Potential of the Synthetic Cannabinoids JWH-073, JWH-081, and JWH-210: In Vivo and In Vitro Approaches

  • Cha, Hye Jin;Lee, Kwang-Wook;Song, Min-Ji;Hyeon, Yang-Jin;Hwang, Ji-Young;Jang, Choon-Gon;Ahn, Joon-Ik;Jeon, Seol-Hee;Kim, Hyun-Uk;Kim, Young-Hoon;Seong, Won-Keun;Kang, Hoil;Yoo, Han Sang;Jeong, Ho-Sang
    • Biomolecules & Therapeutics
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    • v.22 no.4
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    • pp.363-369
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    • 2014
  • Synthetic cannabinoids (CBs) such as the JWH series have caused social problems concerning their abuse liability. Because the JWH series produces euphoric and hallucinogenic effects, they have been distributed illegally under street names such as "Spice" and "Smoke". Many countries including Korea have started to schedule some of the JWH series compounds as controlled substances, but there are a number of JWH series chemicals that remain uncontrolled by law. In this study, three synthetic CBs with different binding affinities to the $CB_1$ receptor (JWH-073, 081, and 210) and ${\Delta}^9$-tetrahydrocannabinol (${\Delta}^9$-THC) were evaluated for their potential for psychological dependence. The conditioned place preference test (unbiased method) and self-administration test (fixed ratio of 1) using rodents were conducted. $K_i$ values of the three synthetic cannabinoids were calculated as supplementary data using a receptor binding assay and overexpressed $CB_1$ protein membranes to compare dependence potential with $CB_1$ receptor binding affinity. All mice administered JWH-073, 081, or 210 showed significantly increased time spent at unpreferred space in a dose-dependence manner in the conditioned place preference test. In contrast, all tested substances except ${\Delta}^9$-THC showed aversion phenomenon at high doses in the conditioned place preference test. The order of affinity to the $CB_1$ receptor in the receptor binding assay was JWH-210 > JWH-081 >> JWH-073, which was in agreement with the results from the conditioned place preference test. However, no change in self-administration was observed. These findings suggest the possibility to predict dependence potential of synthetic CBs through a receptor binding assay at the screening level.

Microbiological and Chemical Detection of Antibiotic Residues in Livestock and Seafood Products in the Korean Market

  • Park, Sung-Kug;Kim, Mee-Hye;Sho, You-Sub;Chung, So-Young;Hu, Soo-Jung;Lee, Jong-Ok;Hong, Moo-Ki;Kim, Myung-Chul;Kang, Ju-Seop;Jhee, Ok-Hwa
    • Food Science and Biotechnology
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    • v.16 no.6
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    • pp.868-872
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    • 2007
  • The microbiological and chemical identification of antibiotic residues was attempted for livestock and seafood products including pork (n=34), beef (n=34), chicken (n=32), flatfish (n=37), armorclad rockfish (n=36), and sea bream (n=27). The meat (n=100) and seafood (n=100) samples were collected from 9 markets in 5 major Korean cities. Antibiotic substances were identified from the classes of tetracyclines, macrolides, penicillins, aminoglycosides, polyethers, peptides, sulfonamides, quinolones, chlorampenicols, and novobiocins using a microbiological assay, the Charm II test and high performance liquid chromatography (HPLC) with ultra violet (UV) and fluorescence detectors. The results showed that 2 tetracyclines (oxytetracycline and tetracycline) and 3 quinolones (ciprofloxacin, norfloxacin, and enrofloxacin) were detected in 4 samples of flatfish among all 100 seafood samples tested. No antibiotic residues were detected in the 100 livestock product samples tested. The amounts (min-max, mg/kg) of the residual antibiotics were as follows; tetracycline 0.78-0.85, oxytetracycline 0.49-0.74, ciprofloxacin 0.09-0.83, norfloxacin 0.01-0.21, enrofloxacin 0.12-2.98. These data indicate that the total detection rate of antibiotics in livestock and seafood products was approximately 2%.