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히드록시프로필인산이전분의 제조조건에 따른 부산물 생성에 과한 연구
조태용,이명자,반경녀,오세동,홍기형,김선봉,최태진,홍무기 식품의약품안전청 2001 식품의약품안전청 연보 Vol.5 No.-
히드록시프로필인산이전분의 안전한 사용과 품질관리를 위하여 propylene chlorohydrin(PCH)의 분석법을 개선하고 생성 정도를 제조조건별로 조사하였다. PCH의 가속용매추출장치(린르도)에 의한 최적 분석조건을 확립하꾸 위하여 추출용매4초산에틸, 메탄올, 아세톤, 헥산 및 에테르), 추출압력(1000~린Oopsi) 및 추출온도(40'E~150'E)를 변화시켜 PCH의 회수율을 검토한 갈과 초산에틸을 추출똥매로 산웅하여 추출압력 2300psi 및 추출온도 120'c로 한였을 때 회수율은 뽄.1 %를 나타내어 PCH 최적 분석 조건으로 하였다. 히드록시프로필인산이전분의 제조조건에 따른 PCH 잔류량을 조사하기 위하여 찰옥수수전분과 옥수 순전분을 사용하여 Propylene oxidefppo) 첨가량(2, 5, 7 및 10%)에 따른 변성정도 및 PC닌함량의 변화들을 조사하였을 때 PPO 첨가량이 증가함에 따라 PC러의 잔류량과 nS(Degree of substituent)가 증가하였는데 찰옥수수전분을 사용한 경우가 옥수수전분에 비해 DS도 높았고 PC보 잔류량도 적었다.히드록시프로필화(fP) 및 가교화fXL)반응의 순저에 따른 DS 및 PCH 잔류량을 조사한 결과 DS는 큰 차이를 나타내지 않았으나 X교-HP의 경우가 PCH 잔류량이 다소 많은 경향을 보였다. 중쑤시약으로 염산, 황산 및 인산을 각각 사용하였글 때 PC또 잔류량은 염산을 사용하였을 경우 가장 높았으나 황산과 인산을 자용한 경우에돈 세척하지 않은 것에서 3.60ppm 및 4.07ppm이 각각 검출되었다. 제조과정 중 잔류하는 PPO을 제거하기 위하여 HP(PPO 10% 첨가)화한 후 은도 45'c를 유지하면서 반응조 뚜껑을 열어 PPO를 휘발시킴과 동시에 완전한 제거를 위하여 질소가스를 200myftn으로 30분간 흘린 후 제조하였을 때 제척하지 않은 경우에도 PCH 잔류량이 Ippm 이하였고 세척한 경우에는 완전히 제거되었다. This study was carried out to improve the analytical method of propylene chlorohydrin(PCH) and to examine the PCH residue by various reaction conditions in the preparation of hydroxypropyl distarch phosphate. By use of ASE(Accelerated Solvent Extractor), the effect of temperature(40∼150℃), pressure(1000∼2500psi) and solvent(ethyl acetate, methanol, aceton, hexane, ether) were investigated to find the optimum conditions which was at 120℃, 2500psi with ethyl acetate. The recovery was above 95% We also examined the PCH residues during the preparation of hydroxypropyl derivatives of waxy corn and corn strch. Degree of substituent(DS) and PCH content were increased with propylene oxide(PPO) level. Modified waxy corn starch had higher DS, lower PCH content than modified corn starch. Effect of DS was no difference between hydroxypropylation(HP) and crosslinking(XL) modification sequence, but the formation of PCH was more affective by XL-HP. When hydrochloric acid as neutralizing reagent was added, PCH residue was the highest. Even though using sulfuric acid and phoshoric acid which have no chloride ion, PCH content each reached to 3.60ppm and 4.07ppm in no washed corn starch. To remove PPO residue after hydroxypropylation, at the same time the reaction temperature(45℃) was maintained, the reaction vessel cover was opened and incorproated nitrogen into starch slurry at the rate of 200ml/min for 30min. In that results, PCH residue was reduced to less than 1ppm which was acceptable, based on Code of Food Additives codex, in no washed modified starches, and after being washed, it was completely removed.
연구보문 : 수질환경 ; 고성능액체크로마토그래피-유도결합플라즈마 질량분석기를 이용한 어류 중 메틸수은 분석법 확립
유경열 ( Kyung Yoal Yoo ),반경녀 ( Kyeong Nyeo Bahn ),김은정 ( Eun Jung Kim ),김양선 ( Yang Sun Kim ),명정은 ( Jyong Eun Myung ),윤혜성 ( Hae Seong Yoon ),김미혜 ( Mee Hye Kim ) 한국환경농학회 2011 한국환경농학회지 Vol.30 No.3
BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine·HCl and heated at 60℃ in microwave for 20 min. Methylmercury in 50 μL of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine·HCl + 0.1% L-cysteine mobile phase at 25℃. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient(r2) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and 0.45 μg/kg respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.
Multi-Pesticide Residue Method for Organopesticide Analysis
Kim, Woo Seong,Lee, Bong Hun,Bahn, Kyeong Nyeo,Jung, Sung Ug,Park, Heung Jai 한국환경과학회 1997 한국환경과학회지 Vol.6 No.4
Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low(0.021-0.058㎎/㎏).
퍼지앤트랩 - 기체크로마토그래피(PT - GC)를 이용한 식품첨가물 중 1,4 - 디옥산 및 클로로히드린류 분석
조태용(Tae Yong Cho),신영민(Yeong-Min Sin),반경녀(Kyeong Nyeo Bahn),오세동(Se Dong Oh),이창희(Chang Hee Lee),이영자(Young Ja Lee),문병우(Byung Woo Moon) 한국식품영양과학회 2003 한국식품영양과학회지 Vol.32 No.7
폴리소르베이트류, 염화콜린, 주석산수소콜린, 변성전분 및 향신료 중 1,4-디옥산 및 클로로히드린류의 분석법을 개발하고 확립된 방법으로 잔류량을 조사한 결과는 다음과 같다. 분석에 사용된 트랩으로는 Vocarb 3000이 적합하였고 이때의 검출한계는 DOX 1.38 μg, EPC 0.23 μg, PCH 3.30 μg, ECH 3.97 μg, DCP 20.43 μg이었다. 검체 온도증가와 무수 황산나트륨 농도 증가에 따라 분석감도는 증가하였으나 60℃ 이상에서는 상대표준편차(RSD, %)가 6%를 초과하여 재현성이 떨어져 분석온도를 50℃로 설정하였다. 폴리소르베이트류에서의 회수율은 염을 첨가하지 않고 측정하였을 때 EPC(66%)를 제외하고는 90%이상을 나타내었다. 염화콜린 및 주석산수소콜린의 경우에는 대부분 회수율이 100% 이상이었으나 주석산수소콜린의 EPC는 20%로 낮게 나타났다. 히드록시프로필인산이전분, 히드록시프로필전분 및 찰옥수 수전분에서는 검체를 가수분해한 후 회수율을 측정한 결과 검체종류별 큰 차이없이 회수율이 90% 이상을 나타내었다. 향신료의 분석에서는 무수황산나트륨을 첨가하여 분석한 결과 회수율이 90%이상이었다. 구매한 폴리소르베이트류, 염화콜린, 주석산수소콜린, 향신료 중 1,4-디옥산 및 클로로히드린류를 분석한 결과 트윈 80에서 DOX가 2.5 ppm 검출되었으나 이 외의 검체에서는 모두 불검출되었고 직접 제조한 히드록시프로필전분에서도 모두 불검출되었다. This study has been performed to develope a method for the simultaneous determination of 1,4-dioxane (DOX), epichlorohydrin (EPC), propylene chlorohydrin (PCH), ethylene chlorohydrin (ECH) and 1,3-dichloro-2-propanol (DCP) in polysorbates, chloline chloride, choline bitartrate, modified starch and spices by purge and trap-gas chromatography. Experimental design was used to select a suitable trap by measuring the limit of detection (LOD) and to investigate the effect of temperature and salt of extraction, and the percentage of recovery in various matrix. The LOD of DOX, EPC, PCH, ECH and DCP were 1.38 μg, 0.23 μg, 3.30 μg, 3.97 μg, 20.43 μg respectively, by means of using Vorcarb 3000 trap with 50℃ sample sparger. Excluding EPC, the recoveries of target compounds were above 90% in all matrix. Target compounds in polysorbates (17), choline chloride (5), choline bitartrate (5), modified starch (8) and spices (25) were not detected. But 2.5 ppm of DOX was detected in Tween 80.
박철우,반경녀,이영남,김정옥,김민석,하영래,Park, Cherl-Woo,Bahn, Kyeong-Nyeo,Lee, Young-Nam,Kim, Jeong-Ok,Kim, Min-Seok,Ha, Yeong-Lae 한국식품영양과학회 2007 한국식품영양과학회지 Vol.36 No.3
The concentrations of conjugated linoleic acid (CLA) in twelve Korean mothers' milk samples collected in October 2006 and four infant formula samples produced by Korean manufacturers were determined. CLA detected from both mothers' milk and infant formula samples was only cis-9, trans-11 CLA isomer. The amount of cis-9, trans-11 CLA in Korean mothers' milk (100 mL) ranged from 4.32 to 10.12 mg ($6.27{\pm}0.28\;mg$). Infant formula (13 g), which is the manufacturers' recommended amount to make up 100 mL with water, contained cis-9, trans-11 CLA isomer in amounts ranging from 1.61 to 2.97 mg ($2.27{\pm}0.31\;mg$). 한국인 모유에는 cis-9, trans-11 CLA 이성체만 동정되었고, 그 함량은 $4.32{\sim}10.12\;mg/100\;mL$(평균 $6.27{\pm}0.28\;mg/100\;mL$)이었고, 지방함량 중에는 $1.35{\sim}3.13\;mg/g$(평균 $1.96{\pm}0.06\;mg/g$)으로 개인에 따라 큰 차이가 있었다. 한국인 모유에 함유된 CLA의 함량은 외국의 CLA 함량에 비해 낮았고, 그 이유는 식사의 차이 때문인 것으로 추정되었다. 국내에서 제조된 조제분유에서도 cis-9, trans-11 CLA만 동정되었는데, 그 함량은 $2.35{\sim}22.82\;mg/100\;g$으로 평균치는 $17.45{\pm}1.24\;mg/100\;g$이었고, 지방에 함유된 cis-9, trans-11 CLA 함량은 $0.45\;mg/g{\sim}0.85\;mg/g$으로 그 평균치는 $0.65{\pm}0.02\;mg/g$이었다. 영유아가 조제분유 제조사의 지시된 13% 조제분유를 섭취할 경우 cis-9, trans-11 CLA를 2.27 mg 섭취하는 것으로 모유 100 mL에 함유되어 있는 양에 비해 낮다. 따라서 조제분유를 조제할 때 모유와 동일한 cis-9, trans-11 CLA를 섭취할 수 있도록 조제분유를 제조하는 것이 바람직하다.