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Structural evaluation of degradation products of Loteprednol using LC-MS/MS: Development of an HPLC method for analyzing process-related impurities of Loteprednol

  • Rajesh Varma Bhupatiraju;Bikshal Babu Kasimala;Lavanya Nagamalla;Fathima Sayed
    • Analytical Science and Technology
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    • v.37 no.2
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    • pp.98-113
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    • 2024
  • The current investigation entails the characterization of five degradation products (DPs) formed under different stress conditions of loteprednol using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In addition, this study developed a stable high-performance liquid chromatography (HPLC) method for evaluating loteprednol along with impurities. The method conditions were meticulously fine-tuned which involved the exploration of the appropriate solvent, pH, flow of the mobile phase, columns, and wavelength. The method conditions were carefully chosen to successfully resolve the impurities of loteprednol and were employed in subsequent validation procedures. The stability profile of loteprednol was exposed to stress degradation experiments conducted under five conditions, and DPs were structurally characterized by employing LC-MS/MS. The chromatographic resolution of loteprednol and its impurities along with DPs was effectively achieved using a Phenomenex Luna 250 mm C18 column using 0.1 % phosphoric acid, methanol, and acetonitrile in 45:25:30 (v/v) pumped isocratically at 0.8 mL/min with 243 nm wavelength. The method produces an accurate fit calibration curve in 50-300 ㎍/mL for loteprednol and LOQ (0.05 ㎍/mL) - 0.30 ㎍/mL for its impurities with acceptable precision, accuracy, and recovery. The stress-induced degradation study revealed the degradation of loteprednol under basic, acidic, and photolytic conditions, resulting in the formation of seven distinct DPs. The efficacy of this method was validated through LC-MS/MS, which allowed for the verification of the chemical structures of the newly generated DPs of loteprednol. This method was appropriate for assessing the impurities of loteprednol and can also be appropriate for structural and quantitative assessment of its degradation products.

Quality Characteristics of Campbell Early added Korean Traditional Wines (Yakju) with Different Yeast and Pretreatment (효모 및 전처리를 달리하여 제조한 캠벨얼리 첨가 약주의 품질 특성)

  • Hyejin Park;Nu Ri Kwon;Jae Eun Park;Hyunman Shin;Ju-Hyoung Kim;Hyun-Ju Eom
    • The Korean Journal of Food And Nutrition
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    • v.37 no.2
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    • pp.57-66
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    • 2024
  • The objective of this study was to investigate the quality characteristics of Campbell Early grape-added traditional Korean wines (yakju) prepared with different yeasts and pretreatments. The first pretreatment (A) was prepared by crushing the grapes, the second method (B) was prepared by heating the grapes at 60~70℃ for 30 minutes, and the third method (C) was prepared by freeze-concentrating grape juice. The pH of the fermented wines ranged from 3.77 to 4.10, and the total acidity of the samples ranged from 0.32 to 0.62%. The a value (redness) ranged from -0.40 to 17.89, which was higher in Campbell Early-added samples than in the controls (grapes not added). Total polyphenol content was the highest in samples prepared by crushing or heating Campbell Early grapes with ES22, and the total flavonoid contents were the highest in samples prepared by crushing Campbell Early grapes with ES22. The anthocyanin contents were also the highest in the samples fermented by heating Campbell Early grapes. ABTS and DPPH radical scavenging activities were also the highest (84.08 and 77.56%, respectively) in samples fermented by heating Campbell Early grapes.

Quality Characteristics and Antioxidant Characteristics of Sword Bean Tea Distributed in Domestic Markets (국내 시중 유통 작두콩차의 품질특성 및 항산화특성)

  • You-jin Park;Eom-ji Hwang;Gyeong-dan Yu;Koan Sik Woo
    • The Korean Journal of Food And Nutrition
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    • v.37 no.2
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    • pp.100-109
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    • 2024
  • This study examined the quality characteristics and antioxidant properties of sword bean tea available in domestic markets. Each product of sword bean tea had distinct appearance characteristics. The color, pH, brownness, and turbidity of the tea varied significantly across different products, with tea bags showing higher levels of brownness and turbidity. The total polyphenol content of hot water extraction ranged from 165.13 to 517.69 mg gallic acid equivalents (GAE)/100 g sample for pod tea, 999.36 to 2,054.74 mg GAE/100 g sample for tea bag tea, and 74.62 to 275.00 mg GAE/100 g sample for grain tea, respectively. Similarly, the total flavonoid content, measured in terms of catechin equivalents (CE), ranged from 39.51 to 65.00 mg CE/100 g sample for pod tea, 86.57 to 253.63 mg CE/100 g sample for tea bag tea, and 32.94 to 38.63 mg CE/100 g sample for grain tea, for hot water extraction. The DPPH and ABTS radical scavenging activities of pod tea were 95.68 to 276.19 mg TE/100 g sample and 270.87 to 804.21 mg trolox equivalents/100 g sample, respectively, for hot water extraction. These results suggest the need to establish quality standards to ensure consistent quality of sword bean tea.

Markerless camera pose estimation framework utilizing construction material with standardized specification

  • Harim Kim;Heejae Ahn;Sebeen Yoon;Taehoon Kim;Thomas H.-K. Kang;Young K. Ju;Minju Kim;Hunhee Cho
    • Computers and Concrete
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    • v.33 no.5
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    • pp.535-544
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    • 2024
  • In the rapidly advancing landscape of computer vision (CV) technology, there is a burgeoning interest in its integration with the construction industry. Camera calibration is the process of deriving intrinsic and extrinsic parameters that affect when the coordinates of the 3D real world are projected onto the 2D plane, where the intrinsic parameters are internal factors of the camera, and extrinsic parameters are external factors such as the position and rotation of the camera. Camera pose estimation or extrinsic calibration, which estimates extrinsic parameters, is essential information for CV application at construction since it can be used for indoor navigation of construction robots and field monitoring by restoring depth information. Traditionally, camera pose estimation methods for cameras relied on target objects such as markers or patterns. However, these methods, which are marker- or pattern-based, are often time-consuming due to the requirement of installing a target object for estimation. As a solution to this challenge, this study introduces a novel framework that facilitates camera pose estimation using standardized materials found commonly in construction sites, such as concrete forms. The proposed framework obtains 3D real-world coordinates by referring to construction materials with certain specifications, extracts the 2D coordinates of the corresponding image plane through keypoint detection, and derives the camera's coordinate through the perspective-n-point (PnP) method which derives the extrinsic parameters by matching 3D and 2D coordinate pairs. This framework presents a substantial advancement as it streamlines the extrinsic calibration process, thereby potentially enhancing the efficiency of CV technology application and data collection at construction sites. This approach holds promise for expediting and optimizing various construction-related tasks by automating and simplifying the calibration procedure.

Anaerobic Digestion Biochemical Sludge Produced from Municipal Sewage Treatment Process (하수처리시설에서 발생된 약품 잉여슬러지의 혐기성 소화 특성)

  • Cho, Sang Sun;Kang, Ho;Lim, Bong Su
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.8
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    • pp.561-569
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    • 2014
  • This study was carried out to get the characteristics of anaerobic digestion for chemical/biological sludge produced from municipal sewage treatment plant for phosphorus. Anaerobic mesophilic batch tests showed that the ultimate biodegradability of waste activated sludge showed 31%, PACl sludge 24%, Alum sludge 26%, respectively. At the S/I 1.0, 75% of total biodegradable volatile solids (TBVS) of waste activated sludge was degraded with an initial rapid decay coefficient, k1 of $0.1129day^{-1}$ and 74% of TBVS of PACl sludge with k1 of $0.0998day^{-1}$, and 76% of TBVS of Alum sludge with k1 of $0.1091day^{-1}$ for 20 days. During the operation of SCFMRs, the 3 reactor (Control, PACl, Alum) pH maintained 6.7~7.0 and the reactor alkalinity maintained 1,800~ 2,200 mg/L as $CaCO_3$. The average biogas production rates of SCFMRs fed with PACl sludge and Alum sludge were 0.089 v/v-d and 0.091 v/v-d, respectively, which was 27~28% lower than that of the control (0.124 v/v-d) at an HRT (hydraulic retention times) of 20 days. And the methane content during the operation ranged 70~76% in 3 reactor. The average TVS removal efficiency of SCFMRs fed with PACl sludge and Alum sludge were 19.6% and 19.9%, respectively, at an HRT of 20 days, which showed 4% lower than that of the control (23.8%). The average BVS removal efficiency of SCFMRs fed with PACl sludge and Alum sludge were 25.8% and 26.9%, respectively, at an HRT of 20 days, which was 8~9% lower than that of the control (34.5%).

Effects of Nitrogen Fertilizers on Growth and Nutrient Uptake of Rice Plants and Chemical Properties of Paddy Soil (질소질(窒素質) 비종(肥種)이 수도(水稻)의 생육(生育)과 양분흡수(養分吸收) 및 토양(土壤)의 화학적(化學的) 성질(性質)에 미치는 영향(影響))

  • Lim, Sun-Uk;Kim, You-Hak
    • Korean Journal of Soil Science and Fertilizer
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    • v.17 no.3
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    • pp.232-241
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    • 1984
  • For the purpose of investigating the effect of chemical composition of nitrogenous fertilizers such as urea, ammonium sulfate, ammonium phosphate(dibasic) and aqua-ammonia on growth, yield, efficiency and chemical properties of paddy soil this study was carried out at the same nitrogen concentration through field experiment. The results obtained was summarized as follows. 1. Nitrogenous fertilizers had an effect on plant height at heading stage, plant weight at harvest and No. of spikelet per panicle of rice plants in decreasing order: Ammonium sulfate > Diammonium phosphate > Urea > Ammonia water. But they didn't effect on culm length, spike length, dry matter weight, No. of grain per spike, ripening ratio and weight of 1000 grains of rice plants. 2. The absorbed amount of nitrogen and that of sulfur and nitrogen availability were highest in ammonium sulfate application and lowest in ammonia water application and these were positively correlated with yield. 3. The influence of nitrogenous fertilizers on nitrogen and sulfur efficiency and translocation efficiency was insignificant but that of ammonium sulfate on nitrogen efficiency was higher than that of the others. 4. The effect of nitrogenous fertilizers on a basic chemical properties of paddy soil experimented such as pH, C.E.C, exchangeable cation and organic matter was insignificant. But the sulfur content of ammonium sulfate application and phosphorous content of diammonium phosphate application were higher than that of the others.

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Clinical findings of severe amniotic fluid aspiration pneumonia and effects of surfactant replacement therapy (중증 양수 흡인성 폐렴의 임상양상 및 폐표면 활성제 보충요법의 효과)

  • Park, Sang Woo;Kim, Chun-Soo;Lee, Sang-Lak;Kwon, Tae-Chan
    • Clinical and Experimental Pediatrics
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    • v.52 no.4
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    • pp.429-434
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    • 2009
  • Purpose : Severe aspiration of the amniotic fluid is known to cause fatal respiratory distress in neonates. We conducted this study to investigate the clinical findings of severe amniotic fluid aspiration pneumonia (AFAP) in neonates and the effect of pulmonary surfactant replacement therapy (SRT). Methods : Retrospective analysis of medical records was conducted on 28 patients who received ventilator care due to severe AFAP in a neonatal intensive care unit over a 7-year period (2000-2006). Patients whose amniotic fluid was contaminated with meconium were excluded. Results : A large number of cases were term infants (82.1%) and infants born by caesarean section (85.7%), and the 1- and 5-min Apgar scores of these patients were $6.5{\pm}1.2$ and $7.5{\pm}1.3$, respectively. Soon after birth, the amount of amniotic fluid sucked out from airway below the vocal cord was $16.0{\pm}10.1$ mL. All patients received SRT with a modified bovine-derived surfactant (120 mg/kg/dose), and one dose was administered in most cases (75%). Compared with pre-SRT, the oxygenation index ($8.0{\pm}9.6$ vs. $18.9{\pm}7.3$) according to ventilator care was a significant improvement at 12 h after SRT (P<0.001). Furthermore, most cases showed radiological improvement for aeration at 12 h post-treatment. Many cases (46.4%) had cardiorespiratory complications, but their final outcomes were excellent (survival rate, 96.4%). Conclusion : AFAP may be an important cause of serious respiratory distress in near-term and term infants, and SRT seems to be an effective adjuvant therapy in mechanically ventilated neonates with severe AFAP.

Chemical Analysis and Sensory Evaluation of Commercial Red Wines in Korea (국내유통 적포도주 일반분석 및 소비자 기호도 조사)

  • Yoo, Ki-Seon;Kim, Ji-Sun;Jin, Qing;Moon, Jin-Seok;Kim, Myoung-Dong;Han, Nam-Soo
    • Korean Journal of Food Science and Technology
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    • v.40 no.4
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    • pp.430-435
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    • 2008
  • The sensory characteristics of imported (two dry, two sweet, and one medium dry wines) and domestic (one sweet wine) red wine were evaluated by 250 panels. The preferences of aroma, color, sweetness, tartness, astringency, and overall acceptability were determined by 5-point just-about-right scale. Among six wines, B sample obtained the highest mean overall acceptability score of 3.67 and its chemical and sensory characteristics were as follow: cherry or strawberry aroma, 9.4 brix, 3.7% of sugar content, pH 3.5, 10% of ethanol, 0.14% of tannin, 5.74 mg/mL of total organic acids, and color of $L(12.04{\pm}0.01)$, $a(33.90{\pm}0.19)$, and $b(8.22{\pm}0.00)$. These results revealed that Korean consumers generally prefer sweet taste to dry one, flat taste to bitter one, and fruity aroma to others. Panels preferred a red wine containing high sugar content of $5{\sim}10%$. On the other hand, panels showed low preference to the wine containing tannin above 0.16%. However, these general trends were slightly varied depending on their ages and consuming frequencies.

Water Quality of Streams and Riparian Vegetation at Rice Cultivation Area of Eastern Jeonnam (벼 재배기간중 전남동부지역 농촌하천의 수질과 분포초종)

  • Lee, Do-Jin;Cho, Ju-Sik;Kuk, Yong-In;Ahn, Ho-Geun
    • Korean Journal of Environmental Agriculture
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    • v.22 no.1
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    • pp.7-15
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    • 2003
  • The characteristic of the quality of stream water and the riparian vegetation during rice cultivation in the rural area of the eastern Jeonnam province was surveyed from April to November, 2000. The water quality of the streams during rice cultivation was variable. The pH of these water bodies ranged from $6.5{\sim}8.3$. Electro conductivity (EC) at each water body ranged from $162{\sim}4,910\;{\mu}S/cm$ for Beogyo-cheoa $114.7{\sim}286.6\;{\mu}g/cm$ for Boseong-cheon, $74.8{\sim}147\;{\mu}S/cm$ for Songgwang-cheon, and $61.6{\sim}82.1\;{\mu}S/cm$ for Isa-cheon. Total nitrogen and other parameters (K, Ca, Mg, Na, $Cl^-$, SS) were higher at May (Boseong-cheon) through June (Songgwang-cheon, Isa-cheon) during the transplanting season than these same parameters at August October and November. Thirty weed species of sixteen families were found in the survey areas of Songgwang-cheon, Boseong-cheon Isa-cheon and Beolgyo-cheon. Nine annual weeds, four biennial weeds, and seventeen perennial weeds were found, several different life forms were identified. Of those species three were submerged, two were free floating, five were emerged, and twenty were water-side weeds.

The Vertical Changes of Zooplankton Dynamics and Community Filtration Rate in the Artificial Lake (Okjeong Lake) (인공호수(옥정호)내 동물플랑크톤 동태 및 군집 여과율의 수직적 변화)

  • La, Geung-Hwan;Lee, Hak-Young;Kim, Hyun-Woo
    • Korean Journal of Environmental Biology
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    • v.26 no.4
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    • pp.392-401
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    • 2008
  • The vertical changes (upper layer: 0$\sim$0.5 m, middle layer: 4$\sim$5 m and lower layer: 8$\sim$10 m) of the limnological variables, zooplankton dynamics and community filtration rate on the phytoplankton were evaluated monthly intervals from November 2004 to June 2007 at the artificiallake (Okjeong Lake). During the study, the annual mean of water temperatures were 15.2$\pm$7.8$^{\circ}C$ (upper layer), 14.5$\pm$7.4$^{\circ}C$ (middle layer) and 13.0$\pm$6.2$^{\circ}C$ (lower layer), respectively (n=30). The vertical variations of most limnological parameters (DO, pH, conductivity and turbidity) were fairly similar, except for chl.-${\alpha}$ concentration. Annual mean of chl.-${\alpha}$ concentration was highest at the upper layer (21.4 ${\mu}g$ L$^{-1}$), while annual means of concentrations were low at the middle layer and lower layer (4.3 ${\mu}g$ L$^{-1}$ and 3.5 ${\mu}g$ L$^{-1}$, respectively). Annual mean of Secchi depth was 261 cm (n=30). A total 45 species of zooplankton were identified (28 rotifers, 12 cladocerans and 5 copepods) during the study. The mean abundance of rotifers was highest (124$\pm$232 ind. L$^{-1}$, n =90) and that of cladocerans and copepods were relatively low (22$\pm$56 ind. L$^{-1}$ and 13$\pm$30 ind. L$^{-1}$) in the whole layer. Total zooplankton abundance increased from late spring to summer, and then declined and remained low throughout the winter. The annual mean of total zooplankton filtration rate for phytoplankton at the lower layer was much higher than that of both layers (upper layer: 44.4$\pm$107.8, middle layer: 95.1$\pm$436.4 and lower layer: 158.2$\pm$436.4 mL L$^{-1}$ day$^{-1}$). Among the major zooplankton community, relative community filtration rate (RCFR, %) of copepods for phytoplankton (50.2$\sim$54.8%) was much higher than that of cladocerans (27.7$\sim$36.3%) and rotifers (8$\sim$17.6%). The seasonal variation of RCFRs of major zooplankton community was observed. The RCFRs of rotifers were high in winter (44.6%, n=9), while the RCFRs of cladocerans were high in summer (58.0%, n=7). In spring and fall, the RCFRs of copepods were high in the whole layer (spring: 67.4%, n=9; fall: 74.4%, n=5).