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A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS (HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구)

  • Lee, Seong-Bong;Yong, Kum-Chan;Hwang, Sun-Il;Kim, Young-Su;Jung, You-Jung;Seo, Mi-Young;Lee, Chang-Hee;Sung, Jin-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.327-333
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    • 2014
  • A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

Cholesterol, Free Amino Acid, Nucleotide-related Compounds, and Fatty Acid Composition of Korean Hanwoo Bull Beef (한우수소의 부위별 Calorie, Cholesterol, 유리아미노산, 핵산관련물질 및 지방산조성)

  • Cho, Soo-Hyun;Kim, Jin-Hyoung;Seong, Pil-Nam;Choi, Yeon-Ho;Park, Beom-Young;Lee, Yeon-Jung;In, Tae-Sik;Chun, Sun-Young;Kim, Yong-Kon
    • Food Science of Animal Resources
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    • v.27 no.4
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    • pp.440-449
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    • 2007
  • This study was conducted to investigate the compositions of different cuts of Hanwoo bull beef. 10 cuts [Abjin (short plate), Bosup (top sirloin), Cheggt (striploin), Dngsim (loin), Guri (chuck tender), Hongduke (eye of round), Moksim (chuck roll), Sulgit (bottom round), Udoon (top round), Yangi(brisket)] were prepared from 10 Hanwoo bulls (-24 month old) slaughtered during 3 consecutive days. There were no significant differences in the calorie contents among the 10 cuts (p<0.05). In cholesterol content, Hongduke was significantly lower (26.74 mg/100 g) and Abjin was significantly higher (31.08 mg/100 g) than the other cuts (p<0.05). Free amino acid analysis revealed that there were high contents of glutamate (94.33-216.36 mg/100 g) and alanine (154.88-200.31 mg/100 g), followed by arginine, phenylalanine and lysine in the 10 cuts. In addition, Abjin, Bosup, Cheggt, Hongduke, Sulgit and Udoon had significantly higher inosine monophosphate (IMP) contents than Dngsim or Moksim (p<0.05). Inosine contents were highest in Bosup and Sulgit, whereas hypoxanthine contents were highest in Guri (p<0.05). Total collagen contents were significantly higher in Abjin followed by Yangi, Guri and Moksim (p<0.05). With regard to fatty acid composition, Dngsim had significantly higher $C_{18:0}$ than the other cuts, and Udoon had significantly higher $C_{20:4n6}$ than the other cuts (p<0.05). Total contents of saturated fatty acids (SFA) were significantly higher in Abjin, Dngsim and Yangi, whereas total contents of unsaturated fatty acids (UFA) were significantly higher in Hongduke than the other cuts (p<0.05).

Studies on the Determination Method of Monascus Pigments in Foods (식품 중 홍국색소의 분석법에 관한 연구)

  • Lee, Tal-Soo;Lee, Young-Ja;Kwon, Yong-Kwan;Park, Jae-Seok;Ko, Hyun-Sook;Sim, Kyu-Chang;Lee, Ju-Yeun;Shin, Jae-Wook;Song, Jee-Won;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.33 no.5
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    • pp.641-644
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    • 2001
  • This study was performed for development of new analytical method of monascus pigments in foods. In this method, analysis of monascus pigment in foods has been carried out by detection of monascin and ankaflavin of the main color component of monascus pigment as indicator compounds. Monascin and ankaflavin were isolated and identified by TLC, HPLC, Prep. HPLC, $^{1}H-NMR$ and Mass spectrophotometer. The analysis of monascin and ankaflavin in foods such as massal, sausage, mixed press ham, mixed fish sausage, semi-dried sausage and syrup was performed by using reverse phase high performance liquid chromatograph with Capcell Pak C18 column at wave length 390 nm. The quantitative results of monascin were as follows : $0.01{\sim}3.31\;{\mu}g/g$ item in massal, $0.05{\sim}0.10\;{\mu}g/g$ in mixed fish sausage, and $0.34{\sim}0.35\;{\mu}g/g$ in semi-dried sausage. But the quantitative results of ankaflavin were as follows: $0.02{\sim}0.89\;{\mu}g/g$ in massal, ankaflavin were not founded in other samples.

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Extractive Nitrogenous Constituents in the Commercial Marine Seasoned-dried Products and Seasoned-dried and Roasted Products (시판 수산조미건제품의 함질소 엑스성분 조성)

  • Park, Choon-Kyu;Park, Jung-Nim
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.370-379
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    • 2002
  • The composition of extractive nitrogenous constituents in four species of commercial marine seasoned-dried products (SDP) and five species of seasoned-dried and roasted products (SDRP) were analyzed. The extractive nitrogen contents were $688{\sim}1,124$ and $756{\sim}1,099\;mg/100g$ in SDP and SDRP extracts. Contents of Free amino acids such as glutamic acid, taurine, arginine, proline, alanine, and histidine were high in all samples. The combined amino acid amounted to $662{\sim}2,248$ and $1,146{\sim}1,821\;mg/100g$ in SDP and SDRP, respectively, which corresponded to 34.5 and 42.5% of the total free amino acid level. ATP and related compounds were $3.69{\sim}7.37$ and $2.17{\sim}8.45\;{\mu}mol/g$ in SDP and SDRP, respectively. Five types of betaines were detected in both specimens although in small amounts. TMAO, TMA, creatine, and creatinine were detected in both samples, however they have same variation in each sample. There was no significant difference in the extractive nitrogenous constituents between SDP and SDRP except in moisture, salinity, and contents of glutamic acid and creatinin (p<0.01).

Laboratory Tests for Trichloroethylene (TCE) and Toluene Remediation in Soil Using Soil Vapor Extraction (토양증기추출(Soil Vapor Extraction)을 이용한 토양 내 Trichloroethylene (TCE)과 Toluene정화 실험)

  • 이민희;강현민
    • Economic and Environmental Geology
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    • v.35 no.3
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    • pp.221-227
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    • 2002
  • Column experiments were performed to evaluate the removal efficiency of soil vapor extraction (SVE) iota TCE (trichloroethylene) and toluene in soil. Homogeneous Ottawa sands and real soils collected from contaminated area were used to investigate the effect of soil properties and SVE operation conditions on the removal efficiency. In column teats with two different sizes of Ottawa sand, the maximum effluent TCE concentration in a coarse sand column was 442 mg/L and 337 mg/L in a fine sand column. However, after 20 liter gas flushing, the effluent concentrations were very similar and more than 90% of initial TCE mass were removed from the column. For two real contaminated soil columns, the maximum effluent concentration decreased 50% compared with that in the homogeneous Ottawa coarse sand column, but 99% of initial TCE mass were extracted from the column within 40 liter air flushing, suggesting that SVE is very available to remove volatile NAPLs in the contaminated soil. To investigate the effect of contaminant existing time on the removal efficiency, an Ottawa sand column was left stable for one week after TCE was injected and the gas extraction was applied into the column. Its effluent concentration trend was very similar to those for other Ottawa sand columns except that the residual TCE after the air flushing showed relatively high. Column tests with different water contents were performed and results showed high removal efficiency even in a high water content sand column. Toluene as one of BTEX compounds was used in an Ottawa sand column and a real soil column. Removal trends were similar to those in TCE contaminated columns and more than 98% of initial toluene mass were removed with SVE in both column.

Characteristics of Groundwater, Sewage Water and Stream Water Contamination Based on VOCs Concentration Around Ulsan, Korea (울산지역 지하수, 하수 및 하천수의 VOCs 오염특성)

  • Cho, Byong-Wook;Yun, Uk;Im, Hyun-Chul;Sung, Ig-Hwan;Jang, Woo-Seog
    • Economic and Environmental Geology
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    • v.38 no.1
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    • pp.57-65
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    • 2005
  • To investigate the characteristics of the volatile organic compounds (VOCs) concentration in the groundwater around Ulsan, Korea, 168 groundwaters, 12 stream waters, and 6 sewage waters were analyzed for 61 VOCs. Results showed that VOCs were not detected in stream waters and total VOCs concentration in 5 sewage waters was in the range of ND-22.3 ${\mu}$g/L. In 78 groundwater samples more than one VOCs were detected and VOCs concentration of the samples ranged from 0.1 ${\mu}$g/L to 387.1 ${\mu}$g/L. However, VOCs concentration of 66 samples out of 78 samples showed less than 10 ${\mu}$g/L and that of only 6 samples exceeded Korea drinking water limit (KDWL). 42 VOCs detected from the 168 groundwaters were 14 aromatic hydrocarbons out of 25, 27 chlorinated aliphatic hydrocarbons out of 35, and methyl tert-butyl ether (MTBE). Detection rate of each VOCs in the groundwaters was as follows: chloroform in 43 samples (25.6%), methylene chloride in 36 samples (21.4%), TCE in 26 samples (15.5%), 1,1-dichloroethane in 19 samples (1.3%), PCE in 16 samples (9.5%), cis-1,2-DCE in 15 samples (8.9%), and toluene in 14 samples (8.3%). Even though VOCs concentration in the groundwaters of the study area is still low, the city is expanding and the drinking water limit is becoming strict, and therefore continuous monitoring is necessary.

Isolation, Purification and Some Properties of Polyphenol Oxidase from Pear (배과실(果實)의 Polyphenol Oxidase의 분리(分離) 정제(精製) 및 그 특성(特性))

  • Kang, Yoon Han;Sohn, Tae Hwa;Choi, Jong Uck
    • Current Research on Agriculture and Life Sciences
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    • v.4
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    • pp.55-64
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    • 1986
  • Polyphenol oxidase in japanese pear (Pyrus communis var. mansamkil) was isolated, partially purified and its some properties were investigated. Polyacrylamide disc gel electrophoresis indicated two bands with polyphenol oxidase activity in the extract from acetone dry powder of par flesh. These two polyphenol oxidases (PPO A and PPO B) were purified through acetone precipitation and diethylaminoethyl cellulose column chromatography. PPO A and B were purified 7.8 fold and 8.7 fold by the present procedure, respectively. The Rm values of partially purified PPO A and B were estimated to be 0.58 and 0.68, respectively. The optimum temp, and pH of PPO A activity were $33^{\circ}C$ and pH 7.0, while those of PPO B were $30^{\circ}C$ and pH 4.2, respectively. Two PPO were unstable over the temperature of $60^{\circ}C$. The substrate specificity of pear PPO showed high affinity toward o-diphenolic compounds, especially catechol in PPO A and chlorogenic acid in PPO B, but inactive toward m-diphenol, p-diphenol and monophenols. PPO A showed affinity toward the trihydroxyphenolic compound. $Zn^{{+}{+}}$ activated the PPO A activity but $Fe^{{+}{+}}$ inhibited PPO B activity, while $Fe^{{+}{+}}$ and $Zn^{{+}{+}}$ activated the PPO B activity, while $Fe^{{+}{+}}$ and $Zn^{{+}{+}}$ activated the PPO B activity but $K^+$, $Mg^{{+}{+}}$, $Ca^{{+}{+}}$ and $Hg^{{+}{+}}$ inhibited at 10mM concentration. $Cu^{{+}{+}}$ activated the enzyme action at low concentrations but inhibited at high concentration. Inhibition studies indicated that L-ascorbic acid, L-cysteine and thiourea were most potent. The Km values of PPO A and PPO B for catechol were 20mM and 14.3mM, respectively.

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Early Changes after Death of Plaice, Paralichthys olivaceus Muscle -1. Relationship between Early Changes after Death and Temperature Dependency- (넙치(Paralichthys olivaceus)육의 사후 조기 변화 -1. 사후 조기 변화와 온도 의존성의 관계-)

  • KIM Yuck-Yong;CHO Young-Je
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.25 no.3
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    • pp.189-196
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    • 1992
  • To know the extension effect of storage temperature on the pre-rigor period of plaice, Paratichthys olivaceus muscle, the relationship between early changes after death and temperature dependency was studied. Killed plaices instantly with spiking at the brain were stored at $-3^{\circ}C,\;0^{\circ}C,\;5^{\circ}C\;and\;10^{\circ}$ used in studying the changes in rigor Index, ATP and its related compounds, lactate contents and K-value. The most shortest onset time of rigor-mortis and full rigor was revealed in the sample stored at $-3^{\circ}C$ among the all samples, where rigor-mortis began at 4hrs after spiking and maximum tension was attained after 28hrs. However, in case of fresh plaice muscle stored at $10^{\circ}C$, the onset of rigor-mortis and full rigor were retarded to 14hrs and 52hrs after spiking. ATP in sample stored at $5^{\circ}C\;and\;10^{\circ}C$ were decomposed slowly than sample at $0^{\circ}C\;-3^{\circ}C $ and within 35hrs storage. The fastest rate and the maximum content of lactate accumulation were showed in sample stored at $-3^{\circ}$ among the all samples. The correlation coefficient(r) between the rate of rigor mortis and ATP breakdown, rigor mortis and lactate accumulation, and ATP breakdown and lactate accumulation were -0.981946, 0.965044, and -0.964728, respectively. Freshness of $-3^{\circ}C$ stored samples was maintained for the longest time compared with other stored samples. The times reached around $20\%$ of K-value were 240hrs for samples stored at $-3^{\circ}C,\;96hrs\;for\;0^{\circ}C\;samples,\;71hrs\;for\;5^{\circ}C\;samples,\;and\;22hrs\;for\;10^{\circ}C$ samples. Samples stored at $-3^{\circ}C,\;and\;0^{\circ}C$ were showed higher temperature dependency on rate of rigor-mortis, ATP breakdown, and lactate accumulation than $5^{\circ}C\;and\;10^{\circ}C$ stored samples, but those samples have a lower temperature dependency on K-value.

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Peptide Properties of Rapid Salted and Fermented Anchovy Sauce Using Various Pretenses 1. Hydrolysis of Anchovy Sauce and Actomyosin by Various Pretenses (단백질 분해효소를 이용하여 제조한 속성 멸치 액젓의 펩티드 특성 1. 단백질 분해효소에 의한 멸치 액젓 및 Actomyosin의 가수분해)

  • KIM In-Soo;CHOI Young-Joon;HEU Min-Soo;CHO Young-Je;IM Yeong-Sun;GU Yeun-Suk;YEO Saeng-Gyu;PARK Jae-Woon
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.32 no.4
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    • pp.481-487
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    • 1999
  • The optimal conditions of enzymatic hydrolysis for preparation of rapid salted and fermented anchovy sauce (SFAS) using various pretenses such as trypsin, chymotrypsin, crude enzyme from squid liver and viscera, Alcalase, Neutrase and Protamex were studied. SFAS prepared with squid viscera had higher level of VBN (173.6 mg/100 g) when stored for 70 days than other samples, and peroxide values were almost equal among all samples during fermentation period. Total amino acids and nonprotein nitrogenous compounds remarkably increased as SFAS treated with Alcalase or Protamex which exhibited higher the hydrolysis rate of $57\%$ at 60 day than others. The optimal pHs of trypsin, chymotryosin, Alcalase, Neutrase and Protamex on anchovy actomyosin were 7.5, 6.5, 6.5, 7.0 and 5.0, respectively. Optimal temperatures of trypsin, chymotryosin, Alcalase and Neutrase were 55, 45, 60 and $55^{\circ}C$, respectively. Otherwise, Protamex activity increased as temperature increased from 20 to $70^{\circ}C$. Protamex had higher $K_m$ (3.545) and $V_{max}$ value (2.688) than others. Protamex affected less by NaCl had $52.5\%$ activity at the fermentation condition of $20^{\circ}C$ and $25\%$ NaCl. Protamex appeared to be very effective for the hydrolysis of crude actomyosin from ancnovy.

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Analytical Validation of Rosmarinic Acid in Water Extract of Perilla frutescens Britton var. acuta Kudo as Functional Health Ingredient (건강기능식품 기능성 원료로써 장흥 차조기 열수 추출물의 지표성분인 로즈마린산 분석법 검증)

  • Park, Sung-Yong;Kim, Jung-Eun;Choi, Chul-Yung;Lee, Dong-Wook;Kim, Ki-Man;Yoon, Goo;Yoon, In-Su;Moon, Hong-Seop;Cho, Seung-Sik
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.1
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    • pp.85-88
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    • 2015
  • This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.