• Title/Summary/Keyword: Recovery of Magnesium

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A study of analytical method for Benzo[a]pyrene in edible oils (식용유지 중 벤조피렌 분석법 비교 연구)

  • Min-Jeong Kim;jun-Young Park;Min-Ju Kim;Eun-Young Jo;Mi-Young Park;Nan-Sook Han;Sook-Nam Hwang
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.291-299
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    • 2023
  • The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R2) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

Study Analysis of Isocycloseram and Its Metabolites in Agricultural Food Commodities

  • Ji Young Kim;Hyochin Kim;Su Jung Lee;Suji Lim;Gui Hyun Jang;Guiim Moon;Jung Mi Lee
    • Korean Journal of Environmental Agriculture
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    • v.42 no.1
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    • pp.71-81
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    • 2023
  • An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C18 column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R2) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Food Characteristics of Protein Isolates Recovered from Olive Flounder Paralichthys olivaceus Roe by Isoelectric Solubilization and Precipitation Process (넙치(Paralichthys olivaceus) 알로부터 등전점 용해/침전공정에 의해 회수한 분리단백질의 식품특성)

  • Sang in Kang;In Sang Kwon;Hyeung Jun Kim;In Seong Yoon;Yu Ri Choe;Jung Suck Lee;Jin-Soo Kim;Min Soo Heu
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.56 no.2
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    • pp.162-173
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    • 2023
  • Four roe protein isolates (RPIs) from olive flounder Paralichthys olivaceus roes (OFR) were recovered by isoelectric solubilization (pH 11 and 12) and precipitation (pH 4.5 and 5.5) and investigated for their food characteristics. RPIs contained 4.5-9.6% moisture, 64.1-69.5% protein, 16.1-19.8% lipid, and 1.0-3.9% ash. The protein yields of RPIs ranged from 50.1 to 56.8%, which was significantly different depending on the recovery conditions. A difference was observed in the SDS-PAGE protein band (25-100 kDa) between the alkaline solubilization at pH 11 (RPI-1 and 2) and pH 12 (RPI-3 and 4). The major amino acids of RPIs were Leu, Lys, Asp, Glu and Ala and major mineral components were sulfur, sodium, phosphorus, and magnesium, which were significantly different from OFR (P<0.05). Additionally, the lead and cadmium content was below the chemical hazard standard of the Korean food standards code. The Hunter color and whiteness of RPIs also showed significant differences according to the treatment conditions of the ISP process (P<0.05). This suggests that protein isolates recovered from olive flounder roes have high potential as nutritional supplements.

Study on congestion of the gills in cultured eels Anguilla japonica III. Effect of NaCl treatment on congestion of the gills in cultured eels, Anguilla japonica (뱀장어 아가미 울혈증에 관한 연구 III. NaCl처리가 울혈증 치료에 미치는 영향)

  • Choi, Min-Soon;Park, Kwan-Ha;Choi, Sang-Hoon;Kim, Young-Gill;Kim, Jong-Myeon;Cho, Jeong-Gon;Jang, Seon-Il
    • Journal of fish pathology
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    • v.8 no.2
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    • pp.111-118
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    • 1995
  • This experiment was carried out in order to elucidate the effect of NaCl(0.85%) acclimation on congestion symptoms in central venous sinuses(CVS) of gill filaments and on the alteration of blood constituents in cultured eels for 1, 2, 3, 4, 5, 6 and 7days after handling stress. After giving a handling stress on eels, the frequency of gill congestion was about 90%. It gradually decreased to 40% on the 3rd day, then increased to 60% on the 7th day in NaCl(0.85%) acclimation. The values of haematocrit(Ht), methemoglobin(Met-Hb), glucose (GLU), calcium($Ca^{++}$), lactic dehydrogenase(LDH), glutamic pyruvic transaminase (GPT) and glutamic oxaloacetic transaminase(GOT) were lower than those of the control, whereas magnesium($Mg^{++}$) and haemoglobin(Hb) were higher than the control. However total protein(Tp) and albumin (ALB) levels similar to the control. When the fish after giving a handling stress were cultured in NaCl-free water as a control, the frequency of gill congestion and the value of blood components showed a similar pattern to that obtained from the NaCl acclimated experiments. However, in the early period(1-3day) after handling stress, NaCl acclimating slightly helped the natural tendancy of recovery. These results suggest that the frequency of gill congestion is not always reduced over the whole period of NaCl acclimation. However, the acclimation to NaCl solution may be a somewhat useful therapy for the gill congestion in stressed eels.

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Column Comparison for the Separation of Ferimzone Z and E Stereoisomers and Development of Trace Residue Analysis Method in Brown Rice Using HPLC-MS/MS (컬럼 비교를 통한 Ferimzone Z 및 E 입체 이성질체의 물질 분리 및 HPLC-MS/MS를 활용한 현미 중 미량잔류분석법 개발)

  • Mun-Ju Jeong;So-Hee Kim;Hye-Ran Eun;Ye-Jin Lee;Su-Min Kim;Jae-Woon Baek;Yoon-Hee Lee;Yongho Shin
    • Korean Journal of Environmental Agriculture
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    • v.42 no.3
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    • pp.203-210
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    • 2023
  • Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C18 and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

Development of Analytical methods for Chinomethionat in Livestock Products (축산물 중 살균제 Chinomethionat의 개별 잔류분석법 확립)

  • Yang, Seung-Hyun;Kim, Jeong-Han;Choi, Hoon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.134-141
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    • 2021
  • BACKGROUND: The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION: The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r2>0.995) in the range of 0.01-0.2 ㎍/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

Electrochemical Characteristics of Dopamine coated Silicon/Silicon Carbide Anode Composite for Li-Ion Battery (리튬이온배터리용 도파민이 코팅된 실리콘/실리콘 카바이드 음극복합소재의 전기화학적 특성)

  • Eun Bi Kim;Jong Dae Lee
    • Korean Chemical Engineering Research
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    • v.61 no.1
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    • pp.32-38
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    • 2023
  • In this study, the electrochemical properties of dopamine coated silicon/silicon carbide/carbon(Si/SiC/C) composite materials were investigated to improve cycle stability and rate performance of silicon-based anode active material for lithium-ion batteries. After synthesizing CTAB/SiO2 using the Stöber method, the Si/SiC composites were prepared through the magnesium thermal reduction method with NaCl as heat absorbent. Then, carbon coated Si/SiC anode materials were synthesized through polymerization of dopamine. The physical properties of the prepared Si/SiC/C anode materials were analyzed by SEM, TEM, XRD and BET. Also the electrochemical performance were investigated by cycle stability, rate performance, cyclic voltammetry and EIS test of lithium-ion batteries in 1 M LiPF6 (EC: DEC = 1:1 vol%) electrolyte. The prepared 1-Si/SiC showed a discharge capacity of 633 mAh/g and 1-Si/SiC/C had a discharge capacity of 877 mAh/g at 0.1 C after 100 cycles. Therefore, it was confirmed that cycle stability was improved through dopamine coating. In addition, the anode materials were obtain a high capacity of 576 mAh/g at 5 C and a capacity recovery of 99.9% at 0.1 C/0.1 C.

Removal Characteristics of Nitrogen and Phosphorus by Struvite Crystallization using Converter Slag as a Seed Crystal (제강전로슬래그를 정석재로 이용한 Struvite 정석반응에 의한 질소와 인의 제거특성)

  • Yim, Soo-Bin
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.9
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    • pp.879-886
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    • 2010
  • This study investigated the removal characteristics of highly concentrated $NH_4$-N and $PO_4$-P by struvite crystallization using converter slag as a seed crystal. The optimal pH range for removal and recovery of $NH_4$-N and $PO_4$-P by struvite crystallization was measured to be 8.0~8.75, in which total removal efficiencies for $NH_4$-N and $PO_4$-P by struvite precipitation and crystallization were 34.3~61.0% and 91.0~96.2%, respectively. The maximum removal efficiencies for $NH_4$-N and $PO_4$-P by struvite crystallization were 29.4% at pH 8.5 and 65.1% at pH 8.0, respectively. The removal efficiency of $NH_4$-N by struvite crystallization decreased with increasing calcium ion concentration. The analysis results of SEM, EDS and XRD exhibited that $NH_4$-N and $PO_4$-P in meta-stable region of struvite crystallization could be eliminated through formation of magnesium ammonia phosphate (MAP) and hydroxyapatite (HAp) on seed crystals by struvite precipitation and crystallization.

Concentration of Vanadium in Jeju Groundwater Using Reverse Osmosis Processes (역삼투 공정을 이용한 제주 지하수의 바나듐 농축)

  • Lee, Ho-Won;Moon, Soo-Hyoung;Ko, Kyung-Soo
    • Membrane Journal
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    • v.18 no.3
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    • pp.241-249
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    • 2008
  • This study is to concentrate vanadium in Jeju groundwater using reverse osmosis processes, and to utilize the concentrate for vanadium water. Groundwater samples were taken from Wahyul, Ayum, and Seogwipo groundwater wells with different in vanadium content each other. Their vanadiuln concentrations were 31.8, 44.5, and 53.0 ppb, respectively. The rejection coefficients of every component in groundwater were increased with the increase of TMP At the TMP of $8 kg_f/cm^2$, the rejection coefficients of vanadium, sodium, potassium, aluminium, iron, and barium were $97.4%{\sim}99.0%,\;97.7%{\sim}97.8%,\;98.0%{\sim}98.3%,\;94.8%{\sim}97.5%,\;88.0%{\sim}96.4.0%$, and $97.9{\sim}98.0%$, respectively. And those of magnesium, calcium, chromium, mauganese, and strontium in three groundwater were more than 99.0% at the same TMP. It was possible that vanadium contents of Wahyul, Ayum and Seogwipo groundwater were concentrated into 58.6, 118.9, and 165.1 ppb, respectively, by 6 stages treatment at the recovery ratio of 15%. And these concentrated water (vanadium water) did not exceed the permissible drinking water standards.

Relation between yield and nutrient contents at various growth stages of hulled barley in fields (포장대맥(圃場大麥)의 생육시기별(生育時期別) 양분농도(養分濃度)와 수량(收量)과의 관계(關係))

  • Park, Hoon
    • Korean Journal of Soil Science and Fertilizer
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    • v.9 no.1
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    • pp.39-45
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    • 1976
  • The content of nitrogen, phosphorus, potassium, calcium and magnesium of hulled barley grown on farmer's field with various N.P.K rates were investigated at various growth stages. Correlation analyses between N.P.K contents and yield and use efficiency of N.P.K and other results were as follows. 1. According to concentration and its change at various growth stages N is similar to K and P, Ca, Mg are similar each other. 2. Yield showed significant positive correlation in most fields with nitrogen content just after thawing. However P and N content were more significantly correlated with yield just before freezing in Kangwon and Chungnam (northern and central province). At the other growth stages negative correlation trend was shown between yield and P, especially K. 3. N.P.K contents in plant increased with the increase of fertilizer rate clearly in early growth stage, and especially in nitrogen, indicating that N was relatively short than P and K in the later stage. N and K contents at various fertilizer rates also indicated a probable competition between them. 4. Fertilizer recovery (use efficiency) decreased in the order of N (55)>K (27)>P (12%) and that of N tended to increase with yield increase. 5. Most effective growth stage for nutritional diagnosis in relation to yield appears to be just after thawing or just before freezing. Nutritional criteria for N.P.K at various growth stages were proposed.

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