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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 ) 한국가축위생학회 2000 韓國家畜衛生學會誌 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.
HPLC를 이용(利用)한 축산식품중(畜産食品中) 잔류(殘留) 설폰아 미드제의 동시분석법(同時分析法) 연구(硏究)
황래홍 ( Lae Hwong Hwang ),김영수 ( Young Soo Kim ),윤은선 ( Eun Sun Youn ),김기근 ( Ki Keun Kim ),이규학 ( Kyu Hak Lee ) 한국가축위생학회 1995 韓國家畜衛生學會誌 Vol.18 No.3
This study was carried out to explore the most sensitive and useful method for simultaneous determination of five sulfa drugs (sulfamethazine, sulfamerazine, sulfamonomethoxine, sulfadimethoxine, sulfaquinoxaline) in livestock productions (pork muscle, bovine muscle, chicken muscle, milk) by HPLC with UV detector and reverse phase column. The results obtained were as follows: 1. For mobile phase acetonitrile-0.01M ammonium acetate (23:77) showed more applicable sensitivity and retention times than acetonitrile-1% acetic acid (23:77). Thus acetonitrile-0.01M ammonium acetate(23:77) selected and applied to the modification test, from which it was found pH 6.75 was the most adequate. 2. Optimal wavelength of UV for SMT(sulfamethazine), SMR(sulfamerazine), SMM(sulfamonomethoxine), SD(sulfadimethoxine), and SQ(sulfaquinoxaline) were 266, 266, 265, 269 and 250nm, respectivery, and that for simultaneous application it was 263nm. 3. The average recovery rate by extractant(chloroform, dichloromethane, chlorform+dichloromethane) in the classic method was not significantly different(p>0.05) but that by chloroform higher than the others. Thus chloroform was found to be adequate as extractant in this classic method. 4. The average recovery rate was 86.5% by the MSPD(matrix solid phase disperse) method, which was significantly higher than that by the classic method(p<0.05). Also the recovery rates by method were significantly different(p<0.05) in accordance with sample and type of drug. The MSPD method was much superior to classic method on clean-up.
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 ) 한국가축위생학회 2002 韓國家畜衛生學會誌 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.
MSPD 방법(方法)에 의한 돈육중(豚肉中) Carbadox와 Olaquindox 분석법(分析法) 연구(硏究)
황래홍 ( Lae Hwong Hwang ),김영수 ( Young Soo Kim ),김기근 ( Ki Keun Kim ) 한국가축위생학회 1996 韓國家畜衛生學會誌 Vol.19 No.2
This study was carried out to determination of carbadox and olaquindox residues in swine tissues by MSPD(matrix solid phase disperse)method. The results obtained were as follows; 1. Optimal wavelengths of UV for carbadox and olaquindox were 310 and 370nm, respectively. 2. Ethyl acetate-Acetonitrile(8:2) was found to be adequate as extractant in this method. 3. The average overall recovery of carbadox at the 0.01, 0.05, and 1.0PPM spike levels was 89.2% and that of olaquindox was 89.9%, and the detection limits were 0.5ng for carbadox and olaquindox.
Sulfamethazine 및 Trimethoprim 이 원유(原乳)의 TTC검사(檢査)에 미치는 영향(影響)에 관한 연구(硏究)
김영수 ( Young Soo Kim ),황래홍 ( Lae Hwong Hwang ) 한국가축위생학회 1992 韓國家畜衛生學會誌 Vol.15 No.2
This study was carried out to investigate the effect of sulfamethazine and trimethoprim on TTC test in raw milk. Ten raw milks which does not contain any antibiotics were collected from milk farms and one hundred twenty raw milks which collected from three raw milk receiving stations and those milk samples were mixed up sulfamethazine and trimethoprim for TTC test. The results were as follows: 1. Positive reactions of TTC test were shown above the concentration of 3,000ppm for sulfamethazine and 10ppm for trimethoprim. 2. When the TTC test was conducted with trimethoprim and sulfamethazine mixture, a pair of the concentration of trimethoprim and sulfamethazine shown to positive reaction were 0.1-2,000ppm, 0.5-1,000ppm, 1.0-250ppm and 2.0-100ppm, respectively. 3. Of 120 raw milk samples tested, 16 samples(13%) were shown quasi-positive reaction when the trimethoprim at the concetration of 2ppm was added in the samples.
고속액체크로마토그라피를 이용한 우유 중 노보비오신 분석에 관한 연구
김현정 ( Hyun Jeong Kim ),황래홍 ( Lae Hwong Hwang ),정지헌 ( Ji Heon Joeng ),윤은선 ( En Sun Yoon ),박노운 ( Noh Woon Park ),한인규 ( In Gyou Han ) 한국가축위생학회 1999 韓國家畜衛生學會誌 Vol.21 No.3
A method for the determination of noboviocin in milk was presented by high performance liquid chromatography(HPLC). The novobiocin in the spiked sample was extracted with methanol and evaporated under vacuum. After evaporating, the residue was mixed with distilled water for 2ml, filtrates with 0.45um acrodisc was injected into HPLC. The results obtained were as follows; 1. The calibration curve of novobiocin was showed constantly linear(r 0.999) in the range of 100~500ng/ml. 2. The mean recovery rate of novobiocin from the spiked milk sample were 88~98%. 3. The coefficients of variation were 2.6~5.8%. 4. The lowest detectable limit of novobiocin was 25ppb.
테트라싸이클린계 잔류항생물질 분석을 위한 전처리방법 비교
김동언 ( Dong Eon Kim ),황래홍 ( Lae Hwong Hwang ),윤은선 ( En Sun Yun ),함희진 ( Hee Jin Ham ),양윤모 ( Yoon Mo Yang ),김창기 ( Chang Gi Kim ),기노준 ( No Jun Ki ),이정학 ( Jung Hark Lee ) 한국가축위생학회 2003 韓國家畜衛生學會誌 Vol.26 No.3
Solid phase extraction(SPE) and matrix solid phase dispersion(MSPD) have been studied as preparation procedures for tetracyclines analysis by high-performance liquid chromatography (HPLC) in meat. The recovery range was 74~98% for SPE, and 72~93% for MSPD at spiked levels of l00ng/g for oxytetracycline(OTC), tetracycine(TC), chlortetracycline(CTC), and doxycycline(DC). The detection limits were 15~78ng/g for SPE and 25~84ng/g for MSPD, respectively. Analytical method was HPLC with UV detector. The purpose of this study was developing a practical, accurate and precise method for rapid extraction and quantitation of tetracycline residues in meat.
정지헌 ( Ji Hun Jung ),황래홍 ( Lae Hwong Hwang ),윤은선 ( En Sun Yun ),김현정 ( Hyun Jung Kim ),한인규 ( In Kyou Han ) 한국가축위생학회 1999 韓國家畜衛生學會誌 Vol.22 No.1
This study was performed to investigate the contents of the heavy metals such as cadmium(Cd), copper(Cu), iron(Fe), lead(Pb) and zinc(Zn) in meat and meat products. For this experiment, each 20 samples of beef and pork were collected at slaughterhouse in Seoul areas and 45 samples of meat products(ham, sausage, processed meat and seasoned meat) were purchased from commercial food markets. The contents of the heavy metals was determined by atomic absorption spectrophotometry from Jan. to Nov. in 1998. The results obtained were summarized as follows 1. In Korean native beef, mean values of the heavy metals(mg/kg) were Pb: 0.14±0.10, Cd: 0.07±0.02, Cu: 1.73±0.95, Zn: 42.82±8.17 and Fe: 67.43±24.18, respectively. 2. In imported beef, mean values of the heavy metals(mg/kg) were Pb: 0.03±0.08, Cd: 0.06±0.02, Cu: 1.41±0.62, Zn: 42.93± 4.95 and Fe: 40.06± 12.77, respectively. 3. In pork, mean values of the heavy metals(mg/kg) were Pb: not detected, Cd: 0.09±0.02, Cu: 1.08±0.23, Zn: 19.49±6.02 and Fe: 30.21±10.51, respectively. 4. In ham, mean values of the heavy metals(mg/kg) were Pb: trace, Cd: trace, Cu:1.19± 0.46, Zn: 13.58±4.99 and Fe: 31.43±11.74, respectively. 5. In sausage, mean values of the heavy metals(mg/kg) were Pb: 0.15±0.34, Cd: 0.08±0.05, Cu: 1.15±0.46, Zn: 13.70±7.13 and Fe: 27.28±15.05, respectively. 6. In processed meat, mean values of the heavy metals(mg/kg) were Pb: 0.08±0.13, Cd: 0.09±0.04, Cu: 1.28±0.60, Zn: 14.72±7.09 and Fe: 24.04±10.33, respectively. 7. In seasoned meat, mean values of the heavy metals(mg/kg) were Pb:1.05±2.21, Cd: 0.13 ±0.03, Cu: 1.06± 0.16, Zn: 17.53± 8.72 and Fe: 26.76± 9.02, respectively.