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박준조 ( Jun Jo Bark ),육지혜 ( Ji Hea Youk ),김휴경 ( Hu Kyoung Kim ),박혜원 ( Hye Won Park ),김인경 ( In Kyung Kim ),이우성 ( Woo Seong Lee ) 한국가축위생학회 2007 韓國家畜衛生學會誌 Vol.30 No.3
This study was conducted two kinds of aims: 1) to modify the analytical methods(conditions) by high performance liquid chromatography-fluorescence detector for the detection of residual ivermectin in raw milk, 2) to provide basic information for the evaluation of standard of the residual ivermectin in raw milk. It could be considerable that negative ion spectra can be better method in the LC/MS analysis for the detection of residues. Characteristic daughter ions were observed in negative ion spectra, however, linear line was not formed in positive ion one. Three Holstein cows (500±10kg) were applied to commercial ointment of ivermectin just one time at the first day of test, and residues in raw milk were examined for 20day after administration. The limit of detection(LOD) was 0.65ng(n=5) by HPLC/FLD, and recovery rates were 87.85%~99.47%. The peak was observed at the 4th day, and residues lasted to the end. Thus ivermectin was prohibited when lactating.
박준조 ( Jun Jo Bark ),금모래 ( Mo Rae Keum ),고광춘 ( Kwahng Choon Koh ),박병옥 ( Byoung Ok Park ),이성식 ( Sung Sik Lee ) 한국가축위생학회 2002 韓國家畜衛生學會誌 Vol.25 No.1
A method was developed to separate, detect and qualify aldicarb, bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur in meats and fruits. Experimental beef and fork samples were fortified with 0.05mg/kg of carbamate pesticides for analysis. Carbamate-detected pear by HPLC fluorescence detector(HPLC/FLS) are extracted with acetonitril and refined by solid phase extraction(SPE) filled with aminopropyl-bonded silca, In the following step, the injected materials into LC/MS are analyzed to result in the fact that bendiocarb, carbaryl, carbofuran, ethiofencarb, methomyl, methiocarb, propoxur presents several sorts of fraction ions following with; [M+H]+, [M+Na]+, [M-CONHCH3]+, [M-OCONHCH3]+. In addition, ethiofencarb presents [M-SCH2CH3] ion distinctive and aldicarb presents [M+Na]+ and [M-OCONHCH3]+ ion which is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur excluding [M+H]+ ion. However, [M-OCONHCH3]+ and [M-OCONHCH3]+ fraction ion charactering carbamate pesticides are detected most efficiently with fragment voltage 50eV. As a result, for quantitative analysis, [M+Na]+ ion is the most decisive ion for detection of aldicarb and [M+H]+ ion is the most decisive fraction ion for pesticides such as bendiocarb, carbaryl, carbofuran, ethiofencarb, methiocarb, methomyl, propoxur. Carbaryl-detected pear by HPLC/FLS are analyzed by LC/MS and the result shows that [M+H]+ and [M-CONHCH3]+ ions charactering carbaryl are detected.
HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법
정봉수 ( Bong Su Jung ),박준조 ( Jun Jo Bark ),금모래 ( Mo Rae Gum ),김인경 ( In Kyoung Kim ),박병옥 ( Byoung Ok Park ),한정희 ( Jeong Hee Han ) 한국가축위생학회 2004 韓國家畜衛生學會誌 Vol.27 No.1
A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography(HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM: EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichioromethane, DCM Ethylacetate(3:1), DCM: EA(9:1). The method of extraction solvent with DCM: ethyl acetate(9:1) was the most excellent(87.7~99.3%) in separation and reappearance. 2. In the LC/MS analysis of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H] and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm 11 and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.
경기 남부지역 HACCP 인증 아이스크림 업체와 미인증 업체의 미생물 관리 수준 비교
배진규 ( Jin Gyu Bae ),전오숙 ( Oh Sook Jeon ),박혜원 ( Hye Won Park ),복민순 ( Min Soon Bok ),양호열 ( Ho Yul Yang ),박준조 ( Jun Jo Bark ),고태오 ( Tae Oh Ko ) 한국동물위생학회 2013 韓國家畜衛生學會誌 Vol.36 No.2
The hazard analysis critical control point (HACCP) system was introduced to the Korean livestock slaughter and product processing business in 1997. Ice cream manufacturers focus on the sterilization process in order to reduce microorganism, so the HACCP-accredited ice cream manufacturers particularly set the sterilization process as critical control point (CCP). Therefore, the microbiological test results on the finished products can be considered as one of the indicators which show the level of microbiological control in the ice cream manufacturers. Accordingly, this study was carried out to examine if there is a meaningful difference in terms of the microbiological control level between the HACCP-accredited and non-accredited ice cream manufacturer groups by comparing aerobic plate count (APC) of ice creams. The mean of APC was 1.68 Log CFU/g in the HACCP-accredited ice cream manufacturer group and 2.59 Log CFU/g in the non-accredited ones respectively and there was a statistically significant difference (P<0.05). The test results suggest that the level of microbiological control in the HACCP-accredited ice cream manufactures is much higher than that of non-accredited ones.
국내산 및 수입산 냉동 송이버섯과 능이버섯의 수분함량과 Drip양 비교
김소망(So-Mang Kim),김경제(Kyeong-Je Kim),조아로(A-Ro Jo),박준기(Jun-Ki Park),조천호(Cheon-Ho Jo),권기성(Kisung Kwon),김중범(Jung-Beom Kim) 한국식품영양과학회 2018 한국식품영양과학회지 Vol.47 No.4
본 연구는 인위적으로 증량된 냉동 송이버섯 및 능이버섯의 유통을 차단할 방안을 모색하고자 냉동 송이버섯 및 능이버섯에 인위적으로 증량된 첨가물과 수분 및 drip양을 실험하였다. 국내산 및 수입산 냉동 송이버섯 및 능이버섯에 대해 첨가물별 정성시험을 실시한 결과 모두 음성으로 나타나 냉동 송이버섯 및 능이버섯의 인위적 증량을 위해 첨가물이 사용되지 않았음을 확인하였다. 냉동 송이버섯의 수분함량은 국내산이 88.54%로 가장 낮았으며, 연길 90.65%, 티베트 92.75%, 운남 94.88%로 시료 간 유의적 차이를 나타내었고, 능이버섯의 수분함량은 중국산 92.37%, 국내산 91.63%로 유의적 차이를 보이지 않았다. 중국산 냉동 송이버섯을 산지별로 확보하여 해동 후 drip%를 측정한 결과 티베트 및 운남산 냉동 송이버섯이 각각 23.13%, 20.07%, 연길산 냉동 송이버섯이 14.51%, 국내산 냉동 송이버섯이 11.65%로 국내산보다 중국산 냉동 송이버섯에서 다량의 drip이 발생하였다. 냉동 능이버섯의 경우 국내산 20.79%, 중국산 22.69%로 두 집단 간 drip양에 유의적 차이가 없었다. 따라서 국내산 냉동 송이버섯보다 유의적으로 높은 수분함량과 drip양을 나타낸 운남 및 티베트산 냉동 송이버섯의 경우 세척 과정 중 장시간 물 침지를 실시하여 인위적 증량을 하였을 가능성이 있는 것으로 판단되었다. 생송이버섯을 각각 0.5에서 24시간까지 물 침지한 후 냉동시켜 해동하였을 때 발생한 drip양을 비교한 결과 대조구의 경우 8.84%, 2시간 침지한 경우 21.42%로 물 침지 시간이 증가함에 따라 drip양이 증가하였다. 생능이버섯을 0.5에서 24시간 동안 각각 물 침지하여 drip양을 측정한 결과 침지 시간이 길어질수록 무게가 유의적으로 증가하였다. 따라서 침지 시간에 따른 drip양 변화를 기반으로 인위적 가수 여부를 판단할 수 있을 것으로 판단되었다. 그러나 중국산 냉동 송이버섯의 경우 수입 시 발생할 수 있는 검역문제를 예방하기 위해 물로 세척한 후 냉동하여 수입하는 특징을 가지고 있어 물 침지를 실시하지 않은 냉동 송이버섯의 drip양을 인위적 증량 판별 기준점으로 선정하기 곤란하다. 따라서 내용량이 표시량보다 20% 이상 부족할 경우 행정처분을 가하는 식품위생법과 2시간 이상 물 침지를 실시하여야 drip양이 20%를 초과하는 본 실험결과 및 송이버섯 세척에 2시간 이상 소요되지 않는 세척공정을 고려하여 drip양 20%를 냉동 송이버섯의 인위적 증량 기준점으로 활용할 수 있을 것으로 판단된다. This study investigated the additives and water content used for artificial weight increase in frozen Tricholoma matsutake and Sarcodon aspratus. No additives were detected in mushrooms based on the additives identification test. Moisture content of domestic frozen T. matsutake was lowest at 88.54%, whereas those of Yanji, Tibet, and Yunnan were found to be 90.65%, 92.75%, and 94.88%, respectively. The drip% of frozen T. matsutake in Tibet, Yunnan, and Yanji were 23.13%, 20.07%, and 14.51%, respectively, whereas drip% of domestic frozen T. matsutake was 11.65%. The drip% of frozen S. aspratus was 20.79% of Korean and 22.69% of Chinese products, with no significant difference between the two groups. It is suspected that long-term water immersion is carried out during the washing process for frozen T. matsutake from Tibet and Yunnan, which showed significantly higher moisture content and drip% than domestic frozen T. matsutake. Artificial water immersion of raw T. matsutake was performed from 0.5 to 24 hours respectively, followed by freezing and thawing to compare the drip amount. As a result of artificial water immersion of T. matsutake, higher than 20% drip percentage was observed 2 hours after water immersion. Considering that water immersion processes do not take longer than 2 hours to wash mushrooms and food hygiene applies administrative measures when the net weight is 20% or less than the stated quantity, we suggest higher than 20% drip percentage to judge the artificial weight increase in frozen T. matsutake.