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소지방 중 잔류농약분석을 위한 액-액분배법과 modified QuEChERS법 비교
김연주 ( Yoen Joo Kim ),최윤화 ( Yoon Hwa Choi ),신방우 ( Bang Woo Shin ),이정학 ( Jung Hark Lee ) 한국동물위생학회 2011 한국동물위생학회지 (KOJVS) Vol.34 No.4
This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of C18 and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3∼5.0 μg/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3∼6.2 μg/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).
김연주 ( Yoen Joo Kim ),김미란 ( Mi Ran Kim ),최태석 ( Tae Suk Choi ),김영섭 ( Young Seob Kim ),이주형 ( Ju Hyoung Lee ) 한국동물위생학회 2013 한국동물위생학회지 (KOJVS) Vol.36 No.4
This study was conducted to determine the content of 7 mycotoxins (aflatoxin B1, B2, G1, G2, M1, ochratoxin A and zearalenone) using LC-MS/MS in pork available on the Korean markets. The analysis was carried out using following conditions; C18 column (2.1×100 mm, 1.7 μm), mobile phase composed of H2O (0.1 mM NH4Ac 0.01% HCOOH):Methanol (0.1 mM NH4Ac 0.01% HCOOH), binary pump at a flow rate of 0.5 mL/min and 2 μL of injection volume, MS/MS detector with ESI positive and negative mode. The quantication of mycotoxins was based on matrix-matched calibration curves with a correlation coefficient in excess of 0.99 for the 7 mycotoxins. The dectection limits were ranged 0.74∼ 2.13 ng/g, with mean recoveries between 73.10∼97.46% except aflatoxin B1 (61.31%). We also monitored mycotoxin residues in 208 pork samples. The test results, mycotoxins were not found except one sample. Ochratoxin A in one sample of the test samples was detected below the quantification limit.
한혜진 ( Hye Jin Han ),김연주 ( Yoen Joo Kim ),이경혜 ( Kyung Hye Lee ),윤민 ( Min Yun ),김영섭 ( Young Seob Kim ),이주형 ( Ju Hyoung Lee ) 한국동물위생학회 2014 한국동물위생학회지 (KOJVS) Vol.37 No.3
This study was conducted to compare the contents of preservatives and general composition on four different types of cheese to provide useful data and information to the consumer. We analyzed preservatives (sorbic acid, benzoic acid, dehydroacetic acid, methyl p-hydroxy benzoate, ethyl p-hydroxy benzoate, propionic acid) and general composition (moisture, protein, fat) from total 102 cheeses which are 46 sliced cheeses, 22 string cheeses, 20 cream cheeses and 14 pizza cheeses. Preservatives were detected from total 14 samples, which are suitable for the authorized limits in Korea. Sorbic acid was detected from 13 samples (197.3¡1,736.1 mg/kg) and propionic acid was detected from 1 sample (362.7 mg/kg). Considering from each type of cheese, cream cheese showed the high detection rate (60%); 12 samples of cream cheese contained sorbic acid. The moisture, protein and fat contents of cheeses were in the ranges of 44.3¡56.8%, 7.2¡24.6% and 19.6¡26.8%. Cream cheese had the highest level of moisture (56.8%) and fat (26.8%), but protein level is very low (7.2%).
축산식품 중 비스테로이드성 항염증 약물의 잔류함량 모니터링
최윤화 ( Yoon Hwa Choi ),김연주 ( Yoen Joo Kim ),신방우 ( Bang Woo Shin ),이정학 ( Jung Hark Lee ) 한국동물위생학회 2011 한국동물위생학회지 (KOJVS) Vol.34 No.3
This study was conducted to determine the content of non-steroidal anti-inflammatory drugs (NSAIDs) in meats available on the Korean markets. The analysis was carried out using following conditions; C18 column (100×2.1 mm, 1.7 μm), mobile phase composed of DW (containing 0.1% formic acid): acetonitrile (containing 0.1% formic acid), binary pump at a flow rate of 0.3 ml/min and 5 μl of injection volume, MS/MS detector with ESI positive mode. The calibration range of five NSAIDs showed linearity (r2≥0.99) at concentration range of 3.125~200 μg/kg. The recoveries in fortified muscle more than 78.7~100.3%. The detection limits for meloxicam, ketoprofen, flunixin, carprofen and tolfenamic acid were 3.5, 1.6, 1.7, 9.8 and 4.8 μg/kg, respectively. We also monitored NSAIDs residue in cattle muscle 51 samples. The test results, NSAIDs were all not founded.
총헤모글로빈 농도를 비침습적으로 측정하기 위한 400 - 2500nm 대역의 흡수 스펙트럼 분석
전계진(Kye Jin Jeon),김연주(Yoen Joo Kim),김수진(Su Jin Kim),김홍식(Hong Sig Kim),윤길원(Gil Won Yoon) 한국센서학회 2001 센서학회지 Vol.10 No.6
Absorption spectra of blood components have been measured for the purpose of predicting the total hemoglobin concentration. We obtained absorption spectra of major blood components from the visible to near-infrared of 400∼2500nm region. In the near-infrared, water is the main absorbing constituent. The amount of water in the sample cell varies depending on the volume of solute concentration(water displacement). We acquired water-compensated spectra by considering the variation of water volume depending on the variation of analyte concentration. Those spectra show inherent absorption peaks of analytes and linearity with respect to concentration. We selected wavelengths for non-invasive measurement of hemoglobin concentration considering the scattering effect of tissue and the interference of other blood components.
LC/MS를 이용한 축산물 중 잔류 마크로라이드계 항생물질 분석법 연구
황래홍 ( Lae Hwong Hwang ),윤은선 ( En Sun Yun ),김연주 ( Yoen Joo Kim ),김동언 ( Dong Eon Kim ),양윤모 ( Yoon Mo Yang ),이정학 ( Jung Hark Lee ),이병동 ( Byung Dong Lee ) 한국동물위생학회 2002 한국동물위생학회지 (KOJVS) Vol.25 No.3
This study was carried out to confirm analytical method of residual macrolides in livestock products by LC/MS. 1. Macrolides were analyzed by LC/MS on XTerra C18 column with 0.1%TFA(trifluoroacetic acid)-methanol in a gradient mode as mobile phase, and that were identified by positive chemical ionization with selective ion monitoring at 50~1000 mass range. 2. Residual macrolides were extracted from tissue with acetonitrile, and the extract is purified with a Sep-pak C18 cartridge, and elute macrolides with 0.1M methanolic ammonium acetate. 3. The procedure confirms the presence of each macrolide at 50㎍/kg in spiked sample.
HPLC를 이용한 축산물중 잔류페니실린 및 클로람페니콜의 동시분석법 연구
황래홍 ( Lae Hwong Hwang ),윤은선 ( En Sun Yun ),김현정 ( Hyun Jung Kim ),김연주 ( Yoen Joo Kim ),정형기 ( Hyeoung Ki Jung ),한인규 ( In Kyou Han ),이병동 ( Byung Dong Lee ) 한국동물위생학회 2000 한국동물위생학회지 (KOJVS) Vol.23 No.1
This study was carried out to simultaneous determination of penicillin G and chloramphenicol in livestock products by HPLC. The results abstained were as follows 1. Penicillin G and chloramphenicol were analyzed by HPLC on symmetry C18 column with acetonitrile-0.1 M phosphate buffer containing 0.0157 M thiosulfate (25: 75) as mobile phase at UV 325nm and 280nm, respectively. 2. Samples were applied to a Sep-pak Cig cartridge, from which eluted penicillin derivatized with 2 M 1,2,4-triazole containing 0.001 M mercuric chloride. 3. The average recovery rates of penicillin G and chloramphenicol were 81.8% and 80.3%, respectively, and the detection limits were 5 ppb (5tg/kg: 7.91U/kg) for penicillin G and chloramphenicol in porcine and bovine muscle.