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Monitoring of arsenic and arsenic species in fish collagen in Korea (국내 유통 어류 콜라겐의 총비소 및 비소화학종 함량 모니터링)

  • Yeo-Jae Shin;Mi-Ra Jang;Eun-Hee Kim;Yun-Hee Kim;Min-Jung Kim;Min-Jung Kim;Jae-Hoon Cha;Mi-Hyun Choi;Seok-Ju Cho;In-Sook Hwang;Yong-Seung Shin
    • Analytical Science and Technology
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    • v.36 no.3
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    • pp.135-142
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    • 2023
  • The total arsenic and 6 arsenic species were investigated in 56 fish collagen products using ICP-MS (Inductively coupled plasma-mass spectrometer) and HPLC-ICP-MS(High performance liquid chromatography-Inductively coupled plasma-mass spectrometer). The mean concentrations of total arsenic and arsenic species were 40.103±81.133 ㎍/kg (N.D.~586.686) and 30.070±50.378 ㎍/kg (N.D.~313.871), respectively. The mean concentration of inorganic arsenic was 24.610±32.706 ㎍/kg (N.D.~129.331), and the As(V) (Arsenate) was the most dominant. The standards and specifications of arsenic have not been established for fish collagen products. Our study presents that arsenic levels are relatively safe compared with not only previous studies but also domestic and international standards. However, in one sample, the total arsenic concentration was 586.686 ㎍/kg, showing the inorganic was 8.119 ㎍/kg, and the DMA was 305.752 ㎍/kg, which was high than the Canadian standard for organic arsenic. In conclusion, it is necessary to monitor arsenic levels consistently and establish standards and specifications of arsenic in fish collagen products to assure consumer safety.

Monitoring of Pesticide Residues in Commonly Consumed Medicinal Agricultural Products (다소비 식·약공용농산물의 잔류농약 실태조사)

  • Hee-Jeong Choi;Yun-Sung Kim;Sang-Tae Kim;Nan-Joo Park;Yu-Mi Choi;Na-Young Yoo;Yoo-Li Han;Jeong-Hwa Seo;Jong-Sung Son;Myoung-Ki Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.112-122
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    • 2023
  • We assessed the pesticide residues in the medicinal agricultural products distributed in Korea. Pesticide residues in 72 samples were analyzed using the QuECheRS method for 339 pesticides, using GC-MS/MS and LC-MS/MS. The pesticide residues were below the maximum residues limit (MRL) in 42 samples (58.3%); however, they exceeded the MRL in 5 samples (6.9%). These included 43 types of pesticides; 20 fungicides and 23 insecticides were detected 75 times and 58 times, respectively. Tebuconazole and carbendazim were the most detected fungicides, each 11 times. The levels of acetamiprid, cadusafos, chlorpyrifos, flubendiamide, fluopyram, and triazophos exceeded the MRL in Gogi berry, Omija, and Reishi mushroom. All of them were positive list system (PLS) items that lacked pesticide residue standards. Therefore, authorities should monitor the distributed medicinal agricultural products.

Evaluation of the Bioequivalence of Two Brands of Naltrexone 50 mg Tablet in Healthy Volunteers

  • Baek, In-Hwan;Yun, Hwi-Yeol;Kang, Won-Ku;Kwon, Kwang-Il
    • Korean Journal of Clinical Pharmacy
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    • v.16 no.1
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    • pp.69-74
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    • 2006
  • 날트렉손은 ${\mu}-opioid$ 수용체에 특이적이고 선택적으로 길항작용을 나타내어 마약이나 마약성 진통제의 강한 의존성 치료에 쓰일 뿐만 아니라, 알코올 의존성 치료에도 쓰이는 약물이다. 본 연구는 날트렉손 제제인 레비아 정 (50 mg tablet, 제일약품) 을 대조약으로 하여 시험약인 명인 제약의 트락손 50 mg정의 생물학적 동등성 평가를 하기 위해 22명의 건강한 지원자를 모집하였다. 지원자를 두 군으로 나누어 1정씩 투여하였고 $2{\times}2$ 교차시험을 실시하였다. 날트렉손의 혈장 중의 농도를 정량하기 위하여 발리데이션된 LC/MS/MS를 사용하였다. 채혈 시간은 투약 전 및 투약 후 0.25, 0.5, 0.75, 1, 1.5, 2, 3, 4, 6, 9, 12 시간에 걸쳐 시행하였다. 생물학적 동등성을 판정하기 위한 파라미터로 12시간까지의 혈장 중 농도 곡선 하 면적$(AUC_{12hr})$과 최고 혈중 농도 $(C_{max})$를 사용하였다. $AUC_{12hr}$의 평균은 $43.45ng{\cdot}hr/ml$ (시험약)과 $43.31ng{\cdot}hr/ml$ (대조약) 으로 관찰되었고, $C_{max}$의 경우 각각 12.01 ng/m1 (시험약)과 12.27 ng/ml (대조약)으로 관찰되었다. $AUC_{12hr}$의 경우 로그변환 한 평균치 차의 90%의 신뢰구간이 log0.95-log1.07이었고, $C_{max}$의 경우 log0.87-log1.14로 계산되어 두 항목 모두 log0.8-log1.25이어야 한다는 식품의약품 안전청과 FDA의 기준을 모두 만족시켰다. 이상의 결과를 종합하면 시험약 트락손 정 50mg 은 대조약 레비아 정 50 mg에 대하여 생물학적으로 동등한 것으로 판정되었다.

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Simultaneous Determination of Aflatoxins and Ochratoxin A in Pork by LC-MS/MS (LC-MS/MS를 이용한 돼지고기 중 총아플라톡신 및 오크라톡신 A 동시분석법 확립)

  • Paek, Ockjin;Park, Songyi;Park, Ki Hun;Kim, Sheen-Hee;Suh, Saejung;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.194-200
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    • 2016
  • Aflatoxins and ochratoxin A (AFTs and OTA) are secondary fungal metabolites produced by several moulds, mainly by Aspergillus flavus by Aspergillus ochraceus and Penicillium verrucosum, and these toxins can be transferred to animals and humans through the ingestion of contaminated feed and food. This study was to develop the analytical method for determination the levels of AFTs ($B_1$, $B_2$, $G_1$ and $G_2$) and OTA in pork. The AFTs and OTA were analyzed simultaneously by electrospray ionization in positive ion mode and mass reaction monitoring (MRM) after solid phase extract (SPE) columns clean-up. Performance characteristics, such as accuracy, precision, linear range, limit of detection (LOD) and quantification (LOQ), were also determined. Matrix-matched standard calibration was used for quantification, obtaining the recoveries in the range of 67.3~108.2% with the relative standard deviations of < 20%. Limits of detection and quantification were also estimated, obtaining the limits of quantification ranged in $0.7{\sim}1.3{\mu}g/kg$. The results of the inter-day study, which was performed with pork samples for 3 days, showed an accuracy of 92.0~109.9%. The precisions (expressed as relative standard deviation values) for the inter day variation were 2.6~17.8%. The method developed in this study was able to carry out the analysis with the satisfactory intensity and accuracy.

A 0.31pJ/conv-step 13b 100MS/s 0.13um CMOS ADC for 3G Communication Systems (3G 통신 시스템 응용을 위한 0.31pJ/conv-step의 13비트 100MS/s 0.13um CMOS A/D 변환기)

  • Lee, Dong-Suk;Lee, Myung-Hwan;Kwon, Yi-Gi;Lee, Seung-Hoon
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.46 no.3
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    • pp.75-85
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    • 2009
  • This work proposes a 13b 100MS/s 0.13um CMOS ADC for 3G communication systems such as two-carrier W-CDMA applications simultaneously requiring high resolution, low power, and small size at high speed. The proposed ADC employs a four-step pipeline architecture to optimize power consumption and chip area at the target resolution and sampling rate. Area-efficient high-speed high-resolution gate-bootstrapping circuits are implemented at the sampling switches of the input SHA to maintain signal linearity over the Nyquist rate even at a 1.0V supply operation. The cascode compensation technique on a low-impedance path implemented in the two-stage amplifiers of the SHA and MDAC simultaneously achieves the required operation speed and phase margin with more reduced power consumption than the Miller compensation technique. Low-glitch dynamic latches in sub-ranging flash ADCs reduce kickback-noise referred to the differential input stage of the comparator by isolating the input stage from output nodes to improve system accuracy. The proposed low-noise current and voltage references based on triple negative T.C. circuits are employed on chip with optional off-chip reference voltages. The prototype ADC in a 0.13um 1P8M CMOS technology demonstrates the measured DNL and INL within 0.70LSB and 1.79LSB, respectively. The ADC shows a maximum SNDR of 64.5dB and a maximum SFDR of 78.0dB at 100MS/s, respectively. The ABC with an active die area of $1.22mm^2$ consumes 42.0mW at 100MS/s and a 1.2V supply, corresponding to a FOM of 0.31pJ/conv-step.

Simultaneous Determination of Aminoglycoside Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 아미노글리코사이드계 항생제 9종의 동시분석 및 적용성 검증)

  • Cho, Yoon-Jae;Choi, Sun-Ju;Kim, Myeong-Ae;Kim, MeeKyung;Yoon, Su-Jin;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.123-130
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    • 2014
  • A simultaneous determination was developed for 9 aminoglycoside antibiotics (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygromycin B, kanamycin, neomycin, spectinomycin, and streptomycin) in meat by liquid chromatography tandem mass spectrometry (LC-MS/MS). Each parameter was established by multiple reaction monitoring in positive ion mode. The developed method was validated for specificity, linearity, accuracy, and precision based on CODEX validation guideline. Linearity was over 0.98 with calibration curves of the mixed standards. Recovery of 9 aminoglycosides ranged on 60.5~114% for beef, 60.1~112% for pork and 63.8~131% for chicken. The limit of detection (LOD) and limit of quantification (LOQ) were 0.001~0.009 mg/kg and 0.006~0.03 mg/kg, respectively in livestock products including beef, pork and chicken. This study also performed survey of residual aminoglycoside antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Aminoglycosides were not found in any of the samples.

Establishment of Pre-Harvest Residue Limits and Residue Characteristics of Penthiopyrad and Pyriofenone in Cucumber (Cucumis sativus L.) Under Greenhouse Condition (시설 내 오이(Cucumis sativus L.) Penthiopyrad 재배 중 및 Pyriofenone의 잔류특성과 생산단계 잔류허용기준 설정)

  • Leem, Su-Bin;Kim, Ji-Yoon;Hur, Kyung-Jin;Kim, Hee-Gon;Hur, Jang-Hyun
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.43-49
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    • 2017
  • BACKGROUND: Greenhouse crops are one of agricultural products consumed largely in Korea. Cucumber is a typical example as main vegetables of greenhouse crops. Thus, pesticide residue analysis is an important requirement to guarantee pesticide safety of cucumber. This work was aim to investigate the residues of penthiopyrad and pyriofenone in cucumber after harvest. METHODS AND RESULTS: Cucumber was subjected to treat with penthiopyrad and pyriofenone at a level of recommended dose 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The samples were extracted with organic solvent by using a homogenizer and purified on solid phase cartridge column followed by LC-MS/MS analysis. The recovery levels of penthiopyrad and pyriofenoneranged from approximately 81 to 93% with the method limit of 0.005 mg/kg and coefficient of variation less than 10%. Penthiopyrad and pyriofenone were detected at a level less than maximum residue limit in cucumber at 10 days before. The half-lives of penthiopyrad and pyriofenone were determined to 2.4 ~ 2.6 days. CONCLUSION: Penthiopyrad and pyriofenone are suggested to use in cucumber 10 days before harvest to reach their levels less than maximum residue limit.

Hazardous Heavy Metal Contents of Mushrooms from Retail Markets in Seoul (서울 지역에서 유통되는 버섯류의 유해중금속 함량 조사에 관한 연구)

  • Cha, Hyun-A;Kang, Soon-Hwa;Choe, Su-Bin;Kim, Hyung-Kook;Kang, Sung-Tae
    • Korean Journal of Food Science and Technology
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    • v.46 no.3
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    • pp.283-287
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    • 2014
  • This study determined the hazardous heavy metal content of mushrooms from markets in Seoul, Korea. One hundred and fifty mushroom samples were digested by the microwave method then the hazardous heavy metal (Pb, Cd, As, Cr, Ni and Hg) content was determined by the inductively coupled plasma-mass spectrometry (ICP-MS) and mercury analyzer. The average values of heavy metals in the samples were as follows: (mean [minimum-maximum], ${\mu}g/kg$); Pb 7.8 (1.9-30.0), Cd 45.3 (0.7-292.4), As 54.6 (24.2-229.3), Cr 42.6 (8.4-334.3), Ni 22.4 (up to 180.4), and Hg 8.9 (2.0-25.0). The contents of hazardous heavy metal in mushrooms were lower than those reported previously and also lower than the Provisional Tolerable Weekly Intake (PTWI) limit prescribed by the FAO/WHO. Thus, it could be suggested that the hazardous heavy metals levels in the mushrooms of retail market were adequately safe for consumption.

Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Development and Validation of Analytical Method for Determination of Fungicide Spiroxamine Residue in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Spiroxamine의 시험법 개발 및 검증)

  • Park, Shin-Min;Do, Jung-Ah;Lim, Seung-Hee;Yoon, Ji-Hye;Pak, Won-Min;Shin, Hye-Sun;Kuk, Ju-Hee;Chung, Hyung-Wook
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.296-305
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    • 2018
  • Spiroxamine, one of fungicides, is used to control powdery mildew in various crops and black yellow sigatoka in bananas. The major strength of spiroxamine is to control powdery mildew in various crops and bananas yellow sigatoka in bananas. The compound has shown a high level of activity, good persistence and crop tolerance. Besides powdery mildew, good control of rust, net blotch and Rhynchosporium diseases been indicated in cereals, together with a complementary activity against Septoria diseases. In 2017, the maximum residue limit (MRL) of spiroxamine established in Korea. According to Ministry of ood and rug afety) regulations, spiroxamine residues defined only parent compound. Thus, a analytical method is needed to estimate the residue level of the parent compound. The objective of this study was to develop and validate analytical method for spiroxamine in representative agricultural commodities. Samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interfering substances. The analyte were quantified and confirmed liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.0005{\sim}0.1{\mu}g/mL$) for the analyte in blank extract with coefficient of determination ($r^2$) > 0.99. For validation purposes, recovery studies will be carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries 70.6~104.6% with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges in the Codex guidelines (CAC/GL40, 2003) and MFDS guidelines. proposed analytical method be used as an official analytical method in the Republic of Korea.