• 제목/요약/키워드: P-optimization

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Characterization of degradation products of the Balsalazide by Mass spectrometry: Optimization of stability-indicating HPLC method for separation and quantification of process related impurities of Balsalazide

  • Chilakabattina Naga Narasimha Babu;Ch. Srinivasa Reddy;Bhagya Kumar Tatavarti;M. Radha Madhavi;Venkateswara Rao Anna
    • Analytical Science and Technology
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    • v.37 no.1
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    • pp.25-38
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    • 2024
  • The study aimed to investigate a novel approach by utilizing liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) to separate, identify and characterize very nominal quantities of degradation products (DPs) of balsalazide along with its process related impurities without isolation from their reaction mixtures. The impurities along with balsalazide were resolved on spherisorb ODS2 (250×4.6 mm, 5.0 ㎛) column at room temperature using 0.2 M sodium acetate solution at pH 4.5 and methanol in the ratio of 55:45 (v/v) as mobile phase pumped isocratically at 1.0 mL/min as mobile phase and UV detection at 255 nm. The method shows sensitive detection limit of 0.003 ㎍/mL, 0.015 ㎍/mL and 0.009 ㎍/mL respectively for impurity 1, 2 and 3 with calibration curve liner in the range of 50-300 ㎍/mL for balsalazide and 0.05-0.30 for its impurities. The balsalazide pure compound was subjected to stress studies and a total of four degradation products (DPs) were formed during the stress study and all the DPs were characterized with the help of their fragmentation pattern and the masses obtained upon LC-MS/MS. The DPs were identified as 3-({4-[(E)-(4-hydroxyphenyl) diazenyl]benzoyl}amino)propanoic acid (DP 1), 4-[(E)-(4-hydroxyphenyl)diazenyl] benzamide (DP 2), 5-[(E)-(4-carbamoylphenyl)diazenyl]-2-hydroxybenzoic acid (DP 3) and 3-({4-[(E)-phenyldiazenyl]benzoyl}amino)propanoic acid (DP 4). Based on findings, it was concluded that, the proposed method was successfully applicable for routine analysis of balsalazide and its process related impurities in pure drug and formulations and also applicable for identification of known and unknown impurities of balsalazide.

Overproduction of Xanthophyll Pigment in Flavobacterium sp. JSWR-1 under Optimized Culture Conditions

  • Jegadeesh Raman;Young-Joon Ko;Jeong-Seon Kim;Da-Hye Kim;Soo-Jin Kim
    • Journal of Microbiology and Biotechnology
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    • v.34 no.3
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    • pp.710-724
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    • 2024
  • Flavobacterium can synthesize xanthophyll, particularly the pigment zeaxanthin, which has significant economic value in nutrition and pharmaceuticals. Recently, the use of carotenoid biosynthesis by bacteria and yeast fermentation technology has shown to be very efficient and offers significant advantages in large-scale production, cost-effectiveness, and safety. In the present study, JSWR-1 strain capable of producing xanthophyll pigment was isolated from a freshwater reservoir in Wanju-gun, Republic of Korea. Based on the morphological, physiological, and molecular characteristics, JSWR-1 classified as belonging to the Flavobacterium species. The bacterium is strictly aerobic, Gram-negative, rod-shaped, and psychrophilic. The completed genome sequence of the strain Flavobacterium sp. JSWR-1 is predicted to be a single circular 3,425,829-bp chromosome with a G+C content of 35.2% and 2,941 protein-coding genes. The optimization of carotenoid production was achieved by small-scale cultivation, resulting in zeaxanthin being identified as the predominant carotenoid pigment. The enhancement of zeaxanthin biosynthesis by applying different light-irradiation, variations in pH and temperature, and adding carbon and nitrogen supplies to the growth medium. A significant increase in intracellular zeaxanthin concentrations was also recorded during fed-batch fermentation achieving a maximum of 16.69 ± 0.71 mg/l, corresponding to a product yield of 4.05 ± 0.15 mg zeaxanthin per gram cell dry weight. Batch and fed-batch culture extracts exhibit significant antioxidant activity. The results demonstrated that the JSWR-1 strain can potentially serve as a source for zeaxanthin biosynthesis.

The study of MDCT of Radiation dose in the department of Radiology of general hospitals in the local area (일 지역 종합병원 영상의학과 MDCT선량에 대한 연구)

  • Shin, Jung-Sub
    • Journal of the Korean Society of Radiology
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    • v.6 no.4
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    • pp.281-290
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    • 2012
  • The difference of radiation dose of MDCT due to different protocols between hospitals was analyzed by CTDI, DLP, the number of Slice and the number of DLP/Slice in 30 cases of the head, the abdomen and the chest that have 10 cases each from MDCT examination of the department of diagnostic imaging of three general hospitals in Gyeongsangbuk-do. The difference of image quality, CTDI, DLP, radiation dose in the eye and radiation dose in thyroid was analyzed after both helical scan and normal scan for head CT were performed because a protocol of head CT is relatively simple and head CT is the most frequent case. Head CT was significantly higher in two-thirds of hospitals compared to A hospital that does not exceed a CTDI diagnostic reference level (IAEA 50mGy, Korea 60mGy) (p<0.001). DLP was higher in one-third of hospitals than a diagnostic reference level of IAEA 1,050mGy.cm and Korea 1,000mGy.cm and two-thirds exceeded the recommendation of Korea and those were significantly higher than A hospital that does not exceed a diagnostic reference level (p<0.001). Abdomen CT showed 119mGy that was higher than a diagnostic reference level of IAEA 25mGy and Korea 20mGy in one-third. DLP in all hospitals was higher that Korea recommendation of 700mGy.cm. Among target hospitals, C hospital showed high radiation dose in all tests because MPR and 3D were of great importance due to low pitch and high Tube Curren. To analyze the difference of radiation dose by scan methods, normal scan and helical scan for head CT of the same patient were performed. In the result, CTDI and DLP of helical CT were higher 63.4% and 93.7% than normal scan (p<0.05, p<0.01). However, normal scan of radiation dose in thyroid was higher 87.26% (p<0.01). Beam of helical CT looked like a bell in the deep part and the marginal part so thyroid was exposed with low radiation dose deviated from central beam. In addition, helical scan used Gantry angle perpendicularly and normal scan used it parallel to the orbitomeatal line. Therefore, radiation dose in thyroid decreased in helical scan. However, a protocol in this study showed higher radiation dose than diagnostic reference level of KFDA. To obey the recommendation of KFDA, low Tube Curren and high pitch were demanded. In this study, the difference of image quality between normal scan and helical scan was not significant. Therefore, a standardized protocol of normal scan was generally used and protective gear for thyroid was needed except a special case. We studied a part of CT cases in the local area. Therefore, the result could not represent the entire cases. However, we confirmed that patient's radiation dose in some cases exceeded the recommendation and the deviation between hospitals was observed. To improve this issue, doctors of diagnostic imaging or technologists of radiology should perform CT by the optimized protocol to decrease a level of CT radiation and also reveal radiation dose for the right to know of patients. However, they had little understanding of the situation. Therefore, the effort of relevant agencies with education program for CT radiation dose, release of radiation dose from CT examination and addition of radiation dose control and open CT contents into evaluation for hospital services and certification, and also the effort of health professionals with the best protocol to realize optimized CT examination.

Enhanced Production of Cellobiase by a Marine Bacterium, Cellulophaga lytica LBH-14, in Pilot-Scaled Bioreactor Using Rice Bran (파이롯트 규모에서 미강을 이용한 해양미생물 Cellulophaga lytica LBH-14 유래의 cellobiase 생산)

  • Cao, Wa;Kim, Hung-Woo;Li, Jianhong;Lee, Jin-Woo
    • Journal of Life Science
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    • v.23 no.4
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    • pp.542-553
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    • 2013
  • The aim of this work was to establish the optimal conditions for the production of cellobiase by a marine bacterium, Cellulophaga lytica LBH-14, using response-surface methodology (RSM). The optimal conditions of rice bran, ammonium chloride, and the initial pH of the medium for cell growth were 100.0 g/l, 5.00 g/l, and 7.0, respectively, whereas those for the production of cellobiase were 91.1 g/l, 9.02 g/l, and 6.6, respectively. The optimal concentrations of $K_2HPO_4$, NaCl, $MgSO_4{\cdot}_{7H2}O$, and $(NH_4)_2SO_4$ for cell growth were 6.25, 0.62, 0.28, and 0.42 g/l, respectively, whereas those for the production of cellobiase were 4.46, 0.36, 0.27, and 0.73 g/l, respectively. The optimal temperatures for cell growth and for the production of cellobiase by C. lytica LBH-14 were 35 and $25^{\circ}C$, respectively. The maximal production of cellobiase in a 100 L bioreactor under optimized conditions in this study was 92.3 U/ml, which was 5.4 times higher than that before optimization. In this study, rice bran and ammonium chloride were developed as carbon and nitrogen sources for the production of cellobiase by C. lytica LBH-14. The time for the production of cellobiase by the marine bacterium with submerged fermentations was reduced from 7 to 3 days, which resulted in enhanced productivity of cellobiase and a decrease in its production cost. This study found that the optimal conditions for the production of cellobiase were different from those of CMCase by C. lytica LBH-14.

Optimization of Culture Conditions for D-Tagatose Production from D-Galactose by Enterobacter agglomerans. (Entrobacter agglomerans에 의한 D-Galactose로부터 D-Tagatose 생산조건의 최적화)

  • 오덕근;노회진;김상용;노봉수
    • Microbiology and Biotechnology Letters
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    • v.26 no.3
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    • pp.250-256
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    • 1998
  • D-Tagatose production from D-galactose was investigated using 35 type strains of American Culture Type Collection (ATCC) and Korean Collection for Type Cultures (KCTC) which have potential to produce D-tagatose. Enterobacter agglomerans ATCC 27987 was selected as a D-tagatose producing strain due to its short fermentation time and high production of D-tagatose. Optimization of the culture conditions for D-tagatose production by E. agglomerans ATCC 27987 was performed. Among various carbon sources, D-galactose was the most effective carbon source for D-tagatose production. As the D-galactose concentration was increased, cell growth and D-tagatose production increased. Effect of nitrogen sources on D-tagatose production was studied. Of inorganic nitrogen sources, ammonium sulfate was effective one for D-tagatose production and yeast extract was the most suitable organic nitrogen nutrient. The concentrations of inorganic compounds such as KH$_2$PO$_4$, K$_2$HPO$_4$, and MgSO$_4$$.$7H$_2$O were also optimized for D-tagatose production. The optimal medium was determined to contain D-galactose of 20 g/l, yeast extract of 5.0 g/l, (NH$_4$)$_2$SO$_4$ of 2.0 g/l, KH$_2$PO$_4$ of 5.0 g/l, K$_2$HPO of 5.0 g/l, and MgSO$_4$$.$7H$_2$O of 5 mg/l. The optimal environmental conditions in a 250-$m\ell$ flask were found to be pH of 6.0, temperature of 30$^{\circ}C$, and agitation speed of 150 rpm. D-tagatose of 0.41 g/l could be obtained in 24 h from 20 g/l D-galactose at the optimal culture condition without induction and cell concentration.

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Optimization of HPLC Method and Clean-up Process for Simultaneous and Systematic Analysis of Synthetic Color Additives in Foods (식품 중 타르색소의 동시분석 및 계통분석을 위한 HPLC 분석조건 및 정제과정 확립)

  • Park, Sung-Kwan;Hong, Yeun;Jung, Yong-Hyun;Lee, Chang-Hee;Yoon, Hae-Jung;Kim, So-Hee;Lee, Jong-Ok
    • Korean Journal of Food Science and Technology
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    • v.33 no.1
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    • pp.33-39
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    • 2001
  • To develop a method for separation process using Sep-pak $C_18$, simultaneous and systematic analysis of 8 permitted and 11 non-permitted synthetic food colors in Korea, optimization of analysis conditions for reverse phase ion-pair high performance liquid chromatography was carried out. For the best result of Sep-pak $C_18$ separation the pH of color standard mixture solution was $5{\sim}6$ and 0.1% HCl-methanol solution were set as eluent. The colors eluated from Sep-pak $C_18$ cartridge were determined and confirmed by high performance liquid chromatography with a photodiode array detector at 420 nm for yellow colors type, at 520 nm for red colors type, at 600 nm for blue and green colors type and at 254 nm for mixed colors. Conditions for HPLC analysis were as follows: column, Symmetry $C_18$ (5 m, 3.9 mm $i.d.{\times}150\;mm$); mobile phase, 0.025 M ammonium acetate (containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (65 : 25 : 10) and 0.025 M ammonium acetate(containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (40 : 50 : 10); flow rate, 1 mL/min. It takes 35 minutes for simultaneaus analysis and 18 minutes for systematic analysis. The detection limits range of each colors were $0.01{\sim}0.05\;{\mu}g/g$.

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Process Optimization of Ginseng Berry Extract Fermentation by Lactobacillus sp. Strain KYH isolated from Fermented Kimchi and Product Analysis (발효 김치로부터 분리한 Lactobacillus sp. Strain KYH를 이용한 진생베리 추출물 최적 발효 공정 확립 및 생성물의 특성 분석)

  • Ha, Yoo-Jin;Yoo, Sun-Kyun;Kim, Mee Ree
    • Journal of the East Asian Society of Dietary Life
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    • v.26 no.1
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    • pp.88-98
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    • 2016
  • The pharmacological effects of ginseng berry have been known to improve psychological function, immune activities, cardiovascular conditions, and certain cancers. It is also known that fermentation improves the bioavailability of human beneficial natural materials. Accordingly, we investigated the optimal fermentation conditions of ginseng berry extract with strain isolated from conventional foods. We also analyzed the fermentation product and its antioxidant activity. The bacterium isolated from fermented kimchi was identified as Lactobacillus sp. strain KYH. To optimize the process, fermentation was performed in a 5 L fermenter containing 3 L of ginseng berry extract at 200 rpm for 72 hr. Under optimized conditions, batch and fed-batch fermentations were performed. After fermentation, organic acids, amino acids, sugars, ginsenosides, and antioxidant activity were evaluated. The optimum fermentation conditions were determined as pH 7.0 and a temperature of $30^{\circ}C$, respectively. After fermentation, the amounts and compositions of organic acids, amino acids, sugars, ginsenosides, and antioxidant activity were altered. In comparing the distribution of ginsenosides with that before fermentation, the ginsenoside Re was a major product. However, amounts of ginsenosides Rb1, Rc, and Rd were reduced, whereas amounts of ginsenosides Rh1 and Rh2 increased. Total phenol content increased to 43.8%, whereas flavonoid content decreased to 19.8%. The DPPH radical scavenging activity and total antioxidant activity increased to 27.2 and 19.4%, respectively.

[Retraction] Characteristics and Optimization of Platycodon grandiflorum Root Concentrate Stick Products with Fermented Platycodon grandiflorum Root Extracts by Lactic Acid Bacteria ([논문 철회] 반응표면분석법을 이용한 젖산발효 도라지 추출물이 첨가된 도라지 농축액 제품의 최적화 연구)

  • Lee, Ka Soon;Seong, Bong Jae;Kim, Sun Ick;Jee, Moo Geun;Park, Shin Young;Mun, Jung Sik;Kil, Mi Ja;Doh, Eun Soo;Kim, Hyun Ho
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.11
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    • pp.1386-1396
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    • 2017
  • The purpose of this study was to determine the optimum Platycodon grandiflorum root concentrate (PGRC, $65^{\circ}Brix$), fermented P. grandiflorum root extract by Lactobacillus plantarum (FPGRE, $2^{\circ}Brix$), and cactus Chounnyouncho extract (Cactus-E, $2^{\circ}Brix$) for preparation of PGRC stick product with FPGRE using response surface methodology (RSM). The experimental conditions were designed according to a central composite design with 20 experimental points, including three replicates for three independent variables such as amount of PGRC (8~12 g), FPGRE (0~20 g), and Cactus-E (0~20 g). The experimental data for the sensory evaluation and functional properties based on antioxidant activity and antimicrobial activity were fitted with the quadratic model, and accuracy of equations was analyzed by ANOVA. For the responses, sensory and functional properties showed significant correlation with contents of three independent variables. The results indicate that addition of PGRC contributed to increased bitterness and acridity based on the sensory test and antimicrobial activity, addition of FPGRE contributed to increased antioxidant activity and antimicrobial activity, and addition of Cactus-E contributed to increased fluidity based on the sensory test, antioxidant activity, and antimicrobial activity. Based on the results of RSM, the optimum formulation of PGRC stick product was calculated as PGRC 8.456 g, FPGRE 20.00 g, and Cactus-Ex 20.00 g with minimal bitterness and acridity, as well as optimized fluidity, antioxidant activity, and antimicrobial activity.

Optimization of sterilization conditions for the production of retorted steamed egg using response surface methodology (반응표면분석을 이용한 레토르트 계란찜의 살균조건 최적화)

  • Cheigh, Chan-Ick;Mun, Ji-Hye;Chung, Myong-Soo
    • Korean Journal of Food Science and Technology
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    • v.50 no.3
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    • pp.331-338
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    • 2018
  • The purpose of this study was to determine the optimum sterilization conditions for the production of retorted steamed egg using response surface methodology. Sterilization processes for eighteen conditions using varying sterilization temperature ($X_1$), time ($X_2$), and method ($X_3$) as the independent variables were carried out through a $3^2{\times}2$ experimental factorial design. Quality evaluations after sterilization included measurements of $F_0$ value ($Y_1$), peak stress ($Y_2$), pH ($Y_3$), color value ($Y_{4-6}$), and organoleptic test [preference for appearance ($Y_7$), overall acceptability ($Y_8$), and preference for texture ($Y_9$) and egg taste ($Y_{10}$)]. Dependent variables ($Y_{1-10}$) of eighteen conditions were more affected by temperature and time than by the sterilization method. Eight factors were selected among the dependent variables as significant factors related to the quality of the steamed egg. Finally, by establishing an optimum range of each dependent variable and contour analysis, the optimum sterilization conditions for the production of steamed egg were determined to be $120^{\circ}C$ for 25 min using a 2-step sterilization process.

Optimization of the Indole-3-Acetic Acid Production Medium of Pantoea agglomerans SRCM 119864 using Response Surface Methodology (반응표면분석법을 활용한 Pantoea agglomerans SRCM 119864의 Indole-3-acetic acid 생산 배지 최적화)

  • Ho Jin, Jeong;Gwangsu, Ha;Su Ji, Jeong;Myeong Seon, Ryu;JinWon, Kim;Do-Youn, Jeong;Hee-Jong, Yang
    • Journal of Life Science
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    • v.32 no.11
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    • pp.872-881
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    • 2022
  • In this study, we optimized the composition of the indole-3-acetic acid (IAA) production medium using response surface methodology on Pantoea agglomerans SRCM 119864 isolated from soil. IAA-producing P. aglomerans SRCM 119864 was identified by 16S rRNA gene sequencing. There are 11 intermediate components known to affect IAA production, hence the effect of each component on IAA production was investigated using a Plackett-Burman design (PBD). Based on the PBD, sucrose, tryptone, and sodium chloride were selected as the main factors that enhanced the IAA production at optimal L-tryptophan concentration. The predicted maximum IAA production (64.34 mg/l) was obtained for a concentration of sucrose of 13.38 g/l, of tryptone of 18.34 g/l, of sodium chloride of 9.71 g/l, and of L-tryptophan of 6.25 g/l using a the hybrid design experimental model. In the experiment, the nutrient broth medium supplemented with 0.1% L-tryptophan as the basal medium produced 45.24 mg/l of IAA, whereas the optimized medium produced 65.40 mg/l of IAA, resulting in a 44.56% increase in efficiency. It was confirmed that the IAA production of the designed optimal composition medium was very similar to the predicted IAA production. The statistical significance and suitability of the experimental model were verified through analysis of variance (ANOVA). Therefore, in this study, we determined the optimal growth medium concentration for the maximum production of IAA, which can contribute to sustainable agriculture and increase crop yield.