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Synthesis of Fe-containing mesoporous silica catalysts for phenol hydroxylation using H2O2
윤상순,최정식,안화승 한국화학공학회 2007 화학공학의이론과응용 Vol.10 No.1
Several Fe-containing mesoporous silica materials were prepared by different synthetic routes. Synthesized materials have iron oxide species located either within the mesoporous silica framework as Si-O-Fe, or nano-sized iron oxide particles (FeOx) inside the pore or mostly on the external surface of a mesoporous silica. Ferric nitrate / chloride salts or iron pentacarbonyl were used as a synthesis reagent depending on the synthesis scheme. Catalysts prepared were characterized by XRD, N2 adsorption-desorption, TEM/SEM, UV-Vis and FT-IR spectroscopies. Catalytic activities were compared by carrying out phenol hydroxylation with hydrogen peroxide as oxidant.
향신료에서 유래되는 안식향산, 소브산, 프로피온산의 함유량 조사
윤상순,이상진,임도연,임호수,이근영,김미경,Yun, Sang Soon,Lee, Sang Jin,Lim, Do Yeon,Lim, Ho Soo,Lee, Gunyoung,Kim, MeeKyung 한국식품위생안전성학회 2017 한국식품위생안전성학회지 Vol.32 No.5
본 연구에서는 향신료 중 천연유래 보존료의 함유량을 조사하기 위하여 안식향산, 소브산 및 프로피온산의 함유량을 분석하였다. 향신료 중 안식향산 및 소브산 함량은 액체크로마토그래프 질량분석기(LC-MS/MS)를 이용하였고, 프로피온산 함량은 가스크로마토그래프 질량분석기(GC-MS)를 이용하였다. 에탄올을 이용하여 용매추출 후원심분리 후 농축하는 방법으로 전처리 방법을 확립하였고, 직선성, 검출한계, 정량한계, 회수율 측정으로 분석방법을 검증하였다. 향신료 493건 수거하여 분석한 결과, 안식향산, 소브산, 프로피온산은 각각 165건, 88건, 398건에서 검출되었다. 안식향산, 소브산, 프로피온산의 검출 범위는 각각 불검출-391.99 mg/L, 불검출-57.70 mg/L, 불검출-188.21 mg/L이었다. 안식향산, 소브산, 프로피온산의 평균 검출량이 가장 높게 나타난 품목은 각각 계피(167.15 mg/L), 바질잎(22.79 mg/L), 백후추(51.48 mg/L)이었다. 본 연구에서 확립된 분석방법은 다양한 향신료를 대상으로 낮은 함량의 천연유래 보존료(안식향산, 소브산, 프로피온산) 분석에 적합한 방법이며, 분석결과는 향신료의 천연유래 보존료 함유량을 알 수 있는 근거자료이다. 따라서, 본 연구의 결과는 향후 식품 검사 시 보존료 사용기준 위반 판정으로 인한 민원제기나 국가간 무역마찰 시 기초자료로 활용될 수 있을 것이다. In this study, we investigated the levels of natural preservatives of benzoic acid, sorbic acid, and propionic acid in spices. The quantitative analysis was performed using high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) for benzoic acid and sorbic acid and gas chromatography-mass spectrometry (GC-MS) for propionic acid. The sample was extracted with ethanol using sonication, then centrifuged and evaporated to dryness and redissolved to 1 mL with ethanol to use for the instrumental analysis. The analytical method was validated based on linearity, recovery, limit of detection (LOD), and limit of quantification (LOQ). This method was suitable to determine low amounts of naturally occurring preservatives (benzoic acid, sorbic acid, and propionic acid) in various spices. Benzoic acid, sorbic acid, and propionic acid were found in 165 samples, 88 samples, and 398 samples, respectively from the total of 493 samples. The concentration of benzoic acid, sorbic acid, and propionic acid were ranged at ND-391.99 mg/L, ND-57.70 mg/L, and ND-188.21 mg/L in spices, respectively. The highest mean levels of benzoic acid, sorbic acid, and propionic acid were found in cinnamon (167.15 mg/L), basil leaves (22.79 mg/L), and white pepper (51.48 mg/L), respectively. The results in this study provide ranges of concentration regarding naturally occurring benzoic acid, sorbic acid, and propionic acid in spices. Moreover, the results may use to the case of consumer complaint or trade friction due to the inspection services of standard criteria for the preservatives of spices.
곡류 및 견과 종실류 중 안식향산, 소브산, 프로피온산의 함유량 조사
윤상순,이상진,임도연,임호수,이근영,김미경 한국식품위생안전성학회 2019 한국식품위생안전성학회지 Vol.34 No.1
This study was aimed at investigating the levels of the natural preservatives of benzoic, sorbic and propionic acids in cereal grains, nuts and seeds. Benzoic and sorbic acid were analyzed by high-performance liquid chro-matography with a diode-array detector (HPLC-DAD) and further confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), whereas propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and further confirmed by gas chromatography-mass spectrometry (GC-MS). Benzoic, sorbic and propionic acids were found in 44, 22, and 550 samples out of 702 samples, respectively. From the total of 702 samples. The con-centrations of benzoic, sorbic and propionic acid were ranged from not detected (ND) to 23.74 mg/L, from ND to 7.90mg/L, and from ND to 37.39 mg/L in cereal grains, nuts and seeds, respectively. The concentration ranges determined in this study could be used as standard criteria in the process of inspecting cereal grains, nuts and seeds for preservatives as well as to address consumer complaints or trade disputes.
G-15 : Phenol hydroxylation using Fe-contained MCM-41 catalysts
윤상순,최정식,안화승 한국화학공학회 2007 화학공학의이론과응용 Vol.10 No.2
A series of Fe-MCM-41 catalyst were prepared by hydrothermal synthesis. Phenol hydroxylation was carried out under a variety of experimental conditions, and the effects of such parameters as reaction temperature, solvent, calcination temperature and amount of oxidant and catalyst. Comparison of hydroxylation activity was also made using TS-1, and other Fe oxide nanoparticles.