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Ionic liquid coated magnetic core/shell CoFe2O4@SiO2 nanoparticles for the separation/analysis of trace gold in water sample

  • Zeng, Yanxia;Zhu, Xiashi;Xie, Jiliang;Chen, Li
    • Advances in nano research
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    • v.10 no.3
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    • pp.295-312
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    • 2021
  • A new ionic liquid functionalized magnetic silica nanoparticle was synthesized and characterized and tested as an adsorbent. The adsorbent was used for magnetic solid phase extraction on ICP-MS method. Simultaneous determination of precious metal Au has been addressed. The method is simple and fast and has been applied to standard water and surface water analysis. A new method for separation/analysis of trace precious metal Au by Magnetron Solid Phase Extraction (MSPE) combined with ICP-MS. The element to be tested is rapidly adsorbed on CoFe2O4@SiO2@[BMIM]PF6 composite nano-adsorbent and eluted with thiourea. The method has a preconcentration factor of 9.5-fold. This method has been successfully applied to the determination of gold in actual water samples. Hydrophobic Ionic Liquids (ILs) 1-butyl-3-methylimidazole hexafluorophosphate ([BMIM]PF6) coated CoFe2O4@SiO2 nanoparticles with core-shell structure to prepare magnetic solid phase extraction agent (CoFe2O4@SiO2@ILs) and establish a new method of MSPE coupled with inductively coupled plasma mass spectrometry for separation/analysis of trace gold. The results showed that trace gold was adsorbed rapidly by CoFe2O4@SiO2@[BMIM]PF6 and eluanted by thiourea. Under the optimal conditions, preconcentration factor of the proposed method was 9.5-fold. The linear range, detection limit, correlation coefficient (R) and relative standard deviation (RSD) were found to be 0.01~1000.00 ng·mL-1, 0.001 ng·mL-1, 0.9990 and 3.4% (n = 11, c = 4.5 ng·mL-1). The CoFe2O4@SiO2 nanoparticles could be used repeatedly for 8 times. This proposed method has been successfully applied to the determination of trace gold in water samples.

Simultaneous Analysis of Mycotoxins and Risk Assessment in Seeds using LC-MS/MS (LC-MS/MS를 이용한 종자류 생약의 곰팡이독소 동시분석 및 위해도 평가)

  • Choi, Eun Jung;Park, Young Ae;Choi, Su Jeong;Jung, Sam Ju;Park, Youn Sun;Hwang, In Sook;Yu, In Sil;Shin, Gi Young
    • Korean Journal of Pharmacognosy
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    • v.51 no.4
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    • pp.270-277
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    • 2020
  • This study analyzed mycotoxins, aflatoxin B1, B2, G1, G2, fumonisin B1, B2, ochratoxin A and zearalenone, using LC-MS/MS and conducted risk assessment on 54 samples of seeds distributed in SeoulYangnyeongsi and the management status of extramural herbal dispensary facility. The matched calibration showed a good linearity as observed in 6 concentration levels(r2>0.999) as a result of method validation applied with Arecae semen. Limits of detection(LOD) and quantification(LOQ) were in the range of 0.02-0.11 ㎍/kg and 0.08-0.34 ㎍/kg, respectively. Recoveries also estimated, ranging from 65.1-99.7% with relative standard deviation(RSD) 0.5-6.3%. As a result of the method on 54 samples, mycotoxins were detected in 16 samples. Among them, two Thujae semen showed a degree of concentration that exceeded the aflatoxin specification. In the risk assessment, the human exposure safety standard values were calculated as ADI(Acceptable Daily Intake) for aflatoxin B1, fumonisin and zearalenone. Ochratoxin A was calculated as PTWI(Provisional Tolerable Weekly Intake). The MOE(Margine of Exposure) of aflatoxin B1 was in the range of 40.36-3536.88. And no items exceeded 100% in %TDI(Tolerable Daily Intake) and %TWI(Tolerable Weekly Intake) of fumonisin, zearalenone and ochratoxin A.

A Study on Pollution Conditions and Management of Sand Flooring Related to Animal Feces - Nitrogen Analysis Method Development - (동물 분변으로 인한 모래 바닥재의 오염실태 및 관리 방안에 관한 연구 - 질소분석방법개발 -)

  • Jeong, Won-Gu;Ha, Ji-Young;Oh, Geun-Chan;Huh, In-Ryang;Choi, Seung-Bong
    • Journal of Environmental Health Sciences
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    • v.46 no.6
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    • pp.646-654
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    • 2020
  • Objectives: Users of parks or children's play facilities have pointed to pets' bowel movements as the most serious problem when using them. In prior studies, a very low detection rate of parasites (eggs) in sand flooring materials has been found. Even though feces have been identified, no parasites (eggs) have been detected. Method: A standard solution of nitrate nitrogen was used to verify the reliability of a new nitrogen analysis method. The linearity, precision, and accuracy of the nitrate nitrogen analysis method were verified. Using this method, the pollution distribution of the sand flooring material and the degree of pollution at each point were investigated. Results: As a result of the verification of the nitrogen analysis method, the linearity was found to be good at r2=0.999 when distilled water is mixed in a standard substance solution. The standard substance additive solution r2=0.968 was found to be good. Precision represented 0.01 to 0.06% RSD for peak height. The recovery rate was 92.4 to 104.0 percent, indicating high accuracy. According to the same method of analysis, the flooring material sand at a general amusement facility with the largest number of concealed spaces was nitrate nitrogen 6.1 times higher than at the entrance of the playground. Also, in a comparison between clean sand and sandy flooring, the average nitrogen concentration of the sand flooring material was 24.4-167 times higher than pure sand. Conclusions: As such, no parasites (eggs) were detected at all points under investigation, but the sand flooring was exposed to animal fecal contamination. Therefore, the management of nitrogenous components should allow accurate identification of animal fecal contamination so that the timing of sand replacement can be managed hygienically and safely.

Study of Simultaneous Analysis of Indicator Components of DTP(Digital Textile Printing) Textile Products Using HPLC-MS/MS - Focusing on Natural Dyes - (HPLC-MS/MS를 활용한 DTP(Digital Textile Printing) 제품의 지표성분 동시분석법 연구 - 천연염료를 중심으로 -)

  • Lee, Wonkyoung;Sung, Eunji;Moon, Joung Ryul;Kim, Miji;Kim, Jonghoon
    • The Korean Fashion and Textile Research Journal
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    • v.23 no.6
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    • pp.844-851
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    • 2021
  • Due to the increase in consumers' interest about well-being, interest in eco-friendly products has been increasing due to the harmful effects of various harmful substances contained in textile products and environmental issues. As a result, natural dyes of less potential risk than synthetic dyes and digital textile printing(DTP) textile products with less environmental pollution are drawing attention. However, due to the lack of evaluation criteria for DTP textile products with natural ink and the nature of many colors are stacked layer by layer for dying, the need for simultaneous analysis is emerging. To evaluate whether the natural dye is derived from natural ingredients, the biocarbon content is analyzed. However, in the case of ink made using natural dyes and DTP textile products using natural ink, it is difficult to analyze the biocarbon content due to the limitation of the presence of a small amount of dye contained therein. In this study, we were shown the possibility of natural derived verification by cross-checking the analytes of natural dyes (Persicaria tinctoria, an indigo dye; Dactylopius coccus, a light red; and Curcum longa L., i.e., turmeric) and natural ink with HPLC-MS/MS. The coefficient of determination was 0.999 or higher, the limit of quantification was 0.647-3.664 ㎍/L and a %RSD of each indicator material was less than 10. Then, the extraction amount of natural dyes for five patterned fabrics was analyzed.

Optimization of Extraction Conditions for Swertiamarin in Swertia japonica Makino (당약의 swertiamarin 분석을 위한 추출조건 최적화)

  • Kim, Tae Hee;Jang, Seol;Lee, Ah Reum;Lee, A Young;Choi, Goya;Kim, Ho Kyoung
    • The Korea Journal of Herbology
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    • v.29 no.1
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    • pp.13-18
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    • 2014
  • Objectives : Iridoid glycoside, swertiamarin is a well known bioactive component found in Swertia japonica Makino (SJ). In this study, we tried to optimize a suitable method which would extract swertiamarin effectively. Methods : Extraction of SJ was carried out by various conditions of time (5 - 60 min), temperature ($30-70^{\circ}C$), solvent (from non-polar to polar), and ratio of solvnet / sample (10 : 1 - 40 : 1) using ultrasonic extractor. Swertiamarin in SJ extracts was quantified by high performance liquid chromatography - Phtodiode array detector (HPLC-PDA) using C18 column and the analytical procedure was validated by evaluation of specificity, range, linearity, accuracy (recovery), precision (intra- and inter day variability), limit of detection (LOD), and limit of quantification (LOQ). Results : An efficient extraction condition for swertiamarin in SJ was optimized using sonicator extraction (temperature $40^{\circ}C$, solvent 20% methanol, solvent / sample (20 : 1), and time 10 min. Analytical procedure was optimized by HPLC-PDA using isocratic solvent system of acetonitrile and water (9 : 91), and the method was validated in regard to linearity (correlation coefficient, $R^2$ > 0.9999), range ($50-1000{\mu}g/mL$), intra- and inter-precision (RSD < 5.0 %), and recovery (99 -103 %). LOD and LOQ were 0.051 and $0.155{\mu}g/mL$, respectively. Conclusion : An optimized method of extraction for swertiamarin in SJ was established through conditions of diverse extraction and the validation result indicated that the method is suited for the determination of swertiamarin in SJ.

Quantitative Analysis of Kynurenic Acid in Chestnut Honey from Different Regions and Method Validation (산지별 밤꿀에 함유된 Kynurenic Acid의 정량 분석과 분석법 검증)

  • Kim, Juree;Kim, Doyun;Lee, Sanghyun
    • Korean Journal of Pharmacognosy
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    • v.53 no.2
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    • pp.111-118
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    • 2022
  • Chestnut honey is a sweet dark-colored honey with a distinct bitter aftertaste. It contains numerous phenolic compounds and alkaloids and is noted for its antioxidant and anti-inflammatory activities. However, it has been established that there are differences in the composition and activity of chestnut honey constituents depending on the region of origin, the sources of which warrant further research. In this study, we analyzed the kynurenic acid (KA) contents in chestnut honey produced in nine different regions in Korea, using high-performance liquid chromatography in conjunction with ultraviolet detection, and validated the analytical method developed. Use of a reverse-phase column and detection at a wavelength of 240 nm were found to be optimal for the detection of KA. Similar evaluation of an optimal method for extracting KA from chestnut honey revealed that extraction using 10% EtOH at 20 times the sample volume over a 6 h period was the most suitable for obtaining a high content of KA. Among the nine regional chestnut honeys assessed, KA content was found to be highest in the "Gongju" sample (1.14 mg/g), followed by that in the "Cheongdo" and "Damyang" samples. Validation of the KA analytical method revealed a good analyte linearity, with a correlation coefficient (r2) of 0.9995, an accuracy of between 92.37% and 107.35%, and good precision (RSD ≤ 1.05%). Our findings in this study, based on a validated quantitative analytical method for KA, could make an important contribution to establishing a data profiling procedure for characterizing chestnut honeys produced in different regions, and may also provide basic data for the identification of functional honey.

Novel stability indicating high-performance liquid chromatography method for the separation and simultaneous quantification of acalabrutinib and its impurities in pharmaceutical formulation

  • Venu Gopal Kamani;Sujatha M;Guna Bhushana Daddala
    • Analytical Science and Technology
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    • v.36 no.1
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    • pp.32-43
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    • 2023
  • This study reports for the first time about a stability indicating RP-HPLC method for qualitative and quantitative determination of acalabrutinib in bulk and dosage form and in presence its impurities 1, 2 and 3. The chromatographic separation was carried on Zorbax XDB-C18 (250×4.6 mm; 5 µ id) as stationary phase, Phosphate buffer pH 6.4 and methanol 80:20 (v/v) as mobile phase at a flow rate of 1.0 mL/min, UV detection was carried at wavelength of 238 nm and the analysis was completed with a run time of 15 min. In these conditions the retention time of acalabrutinib and its impurities 1, 2 and 3 was observed to be 3.50, 4.83, 8.40 and 9.93 min respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50 %, 100 % and 150 % was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for acalabrutinib and both impurities studied and the % RSD in each spiked level was found to be less than 2. Stability tests were done through exposure of the analyte solution to five different stress conditions i.e expose to 1N hydrochloric acid, 1 N sodium hydroxide, 3 % peroxide, 80 ℃ temperature and UV radiation at 254 nm. In all the degradation condition, standard drug acalabrutinib was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis there is no other chromatographic detection of other impurities and formulation excipients. Hence the developed method was found to be suitable for the quantification of acalabrutinib and can separate and analyse impurities 1 and 2.

Analysis for explosives in contaminated soil using the electrochemical method (폭발물 오염토양에서 전기화학법을 이용한 RDX 흔적량의 분석)

  • Ly, Suw Young
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.129-134
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    • 2008
  • Cyclic voltammetry (CV) and square wave stripping voltammetry (SW) analysis of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) using the double-stranded ds calf thymus (DNA) mixed in carbon nanotube paste electrode (PE) were provided. The optimum analytical conditions were determined and the peak potential was 0.2 V vs. Ag/AgCl. The linear working ranges of CV (50-75 ug/L) and SW (5-80 ng/L) were obtained. The precisions of RSD in the 10 ug/L was 0.086% (n=15) and the detection limit was 0.65 ng/L ($2.92{\times}10^{-12}M$) (S/N=3) with 300 s adsorption time at the optimum condition. The method was used to determine the presence of explosive chemicals in contaminated soil samples.

Aluminum in rocks: Optimized microwave-assisted acid digestion and UV-Vis spectrophotometric measurement

  • Nguyen Thanh-Nho;Thai Huynh-Thuc;Le-Thi Anh-Dao;Do Minh-Huy;Le-Thi Huynh-Mai;Le Quang-Huy;Nguyen-Thi Kim-Sinh;Nguyen Cong-Hau
    • Analytical Science and Technology
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    • v.36 no.5
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    • pp.216-223
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    • 2023
  • Aluminium (Al) is one of the major elements in rocks and its concentration can be varied, depending on different rock types as well as sources. The present study aimed to propose an analytical method based on the UV-Vis as a cheap, simple, and common instrument equipped in most laboratories for Al quantification in rocks after the microwave assisted acid digestion. The aluminone and 8-hydroxyquinoline were investigated for the colorimetric assay. The results show that the 8-hydroxyquinoline reagent was more favorable in terms of the minimized affects of the potential interferences present in the digested solutions, i.e., Fe3+, Si4+ and F-. The calibration curve was constructed from 0.10 mg/L to 3.00 mg/L with the goodness of linearity (R2 = 0.9996). The limits of detection and quantification (LOD and LOQ) were estimated, i.e., 0.029 mg/L and 0.087 mg/L, respectively. The 8-hydroxyquinoline was applied to real rock samples, demonstrating favorable precision (RSD = 0.34 %-1.8 %) and no remarkable differences were found compared to the inductively coupled plasma-mass spectrometry (ICP-MS) as a reference measurement approach.

Optimization and Bioassay Guided Comparative Techniques for Efficient Extraction of Lutein Esters from Tagetes erecta (Var. Pusa Narangi Genda) Flowers

  • Kawar Lal Dabodhia;Brijesh Tripathi;Narendra Pal Lamba;Manmohan Singh Chauhan;Rohit Bhatia;Vivek Mishra
    • Mass Spectrometry Letters
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    • v.15 no.1
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    • pp.40-48
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    • 2024
  • Capacity of the analytical/quantitative evaluation techniques to satisfy both qualitative and quantitative considerations for effective extraction of marigold oleoresins/xanthophylls and their potential as anti-mycotic and antioxidant activity was assessed. Accelerated solvent extraction (ASE), Soxhlet extraction (SE), Supercritical fluid extraction (SCFE), Cold extraction (CE), and ultrasonically assisted extraction (USE) techniques were evaluated for extraction of oleoresin/xanthophyll content from Tagetes erecta (Var. Pusa Narangi Genda) with respect to solvent consumption, extraction time, reproducibility, and yield. Followed by the antifungal and antioxidant activity evaluation. The overall yield of Tagetes oleoresin was higher in ASE (64.5 g/kg) followed by SE (57.3 g/kg), USE (50.7 g/kg), SCFE (45.3 g/kg) and CE (31.6 g/kg). The lutein esters represented more than 80% of the constituents. Further, xanthophyll/ lutein content in oleoresin was found to be quite higher in HPLC (r2 = 0.996) analysis than in the AOAC recommended UV spectrophotometer analysis. The oleoresin exhibited moderate antioxidant activity (DPPH assay) and antifungal activity against three phytopathogenic fungi. Based on the various parameters, the reproducibility of ASE was better (0.3-8.0%) than that of SE (0.5-12.9%), SCFE (0.2-9.4%), USE (0.3-12.4%) and CE (0.8-15.3%). ASE with (RSD 1.6%) is preferred being faster, reproducible, uses less solvent, robust and automation allows sequential extraction of the sample in less time.