• Title/Summary/Keyword: liquid recovery

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Development of Simultaneous Analysis Method for Dimenhydrinate Containing Complex Pharmaceuticals Using RP-HPLC (고성능 역상 액체 크로마토그래피(RP-HPLC)를 이용한 Dimenhydrinate 함유 복합제제의 동시분석법 개발)

  • Keun-Sik Shin;Jin-Young Park;Jae-Ho Sim
    • The Journal of the Convergence on Culture Technology
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    • v.10 no.5
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    • pp.775-780
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    • 2024
  • In this study, a simultaneous analysis method was developed using reversed-phase high-performance liquid chromatography(RP-HPLC) for the main components of motion sickness medication: Dimenhydrinate, Caffeine, Methyl Paraben, and Propyl Paraben. The analysis was conducted after pretreating the four components, utilizing a C18 column with Acetonitrile and H2O as the mobile phase. UV detection was carried out at a wavelength of 254nm. As a result of the experiment, the values of Resolution(Rs) was well over Rs > 1.5, which indicates that the separation of the four components was efficient. Additionally, the symmetry factor of the components was 0.989, 1.120, 1.256, and 1.280, respectively, showing their symmetrical stability. In the stability assessment, the calibration curves for the four components showed excellent linearity with R2 > 0.9991 to 0.9998. Furthermore, the limit of detection(LOD) ranged between 0.017 to 3.060㎍/ml, while the limit of quantification(LOQ) ranged between 0.050 to 9.180 ㎍/ml. The recovery rates range from 98.28% to 101.71%, and repeatability showed precision within the range of 0.447 to 0.550, and robustness confirmed values with %RSD < 2. The quantitative analysis results of this study demonstrated the effectiveness of a simultaneous analysis method for motion sickness medication components.

Livestock Manure Nutrients Flow Analysis of Integrated Crop-Livestock Farming Model Reflecting the Regional Characteristics (지역특성을 고려한 경축순환농업 모형의 가축분뇨 양분 흐름분석)

  • Lee, Joon Hee;Choi, Hong Lim
    • Journal of the Korea Organic Resources Recycling Association
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    • v.23 no.2
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    • pp.36-46
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    • 2015
  • Integration of crop-livestock farming has been a problem-solving mode for abatement of environmental pollution and recovery of resources in recent years. The objectives of this study were 1) to suggest the customized integration of crop-livestock farming model reflecting the regional characteristics through in-depth analysis of case study and 2) to analyze the livestock nutrients flow in terms of three primary elements as nitrogen(N), phosphorous(P), and potassium(K). The personal interview and survey were carried out in 2012 for a total of 161 farms from four different regions(NS, NW, JJ, YC) in South Korea. The mass balance analysis was used to suggest and evaluate the models for two sites(JJ and YC). The results showed that NS and NW sites produced relatively more livestock manure than the sites of YC and JJ because of the regional differences in livestock numbers and urbanization. The models were suggested for the site JJ and site YC, and 'two track model(energy and resource recovery)' and 'dispersal type model' were assigned respectively. For the nutrient flows, the releasing P and K with new models had increased up to 7%, while N release had decreased down to 15% in both YC and JJ sites compared to the present treatment system. Estimated value showed that there was oversupply of N (719 ton/yr) and $P_2O_5$ (1,269 ton/yr) in YC and deficiency of N (671 ton/yr) and excessive $P_2O_5$ (32 ton/yr) in JJ respectively. Therefore, P runoff has to be considered an eutrophication occurs in rural small stream when an integration of crop-livestock farm system is applied into both sites.

Analysis of Four Pesticides, Isoproturon, Phenmedipham, Pyridate and Nitenpyram Residues by High-Performance Liquid Chromatography with Diode-Array Detector (HPLC를 이용한 Isoproturon, Phenmedipham, Pyridate 및 Nitenpyram 4종 성분의 잔류농약 분석법 개발)

  • Yang, Sung-Yong;Koo, Yun-Chang;Wang, Zeng;Heo, Kyeong;Kim, Hyeong-Kook;An, Eun-Mi;Shin, Han-Seung;Lee, Jin-Won;Lee, Kwang-Won
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.8
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    • pp.1165-1170
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    • 2010
  • A method for the determination of four pesticide compounds, urea (isoproturon), bis-carbamate (phenmedipham), thiocarbamate (pyridate) and vinyllidenediamine (nitenpyram) were examined and analyzed by HPLC with C-18 column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size). Mobile phase consisted of deionized water, acetonitrile and 50 mM $KH_2PO_4$ (pH 2.5). Isoproturon and phenmedipham analytical condition was isocratic elution of the column with 50% solvent A (acetonitrile) and 50% solvent B (deionized water); pyridate was 85% solvent A (acetonitrile) and 15% solvent B (deionized water) at a flow rate of 1 mL/min; and nitenpyram analytical condition was 90% solvent A (50 mM $KH_2PO_4$, pH 2.5) and 10% solvent B (acetonitrile) at a flow rate of 1 mL/min. In results, retention times were 6.12, 8.63, 9.40 and 12.76 min for isoproturon, phenmedipham, pyridate and nitenpyram, respectively. All injection volumes were $10\;{\mu}L$ and the limit of quantitation was 0.05 mg/kg for four pesticide compounds, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four pesticide compounds were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 70.18% to 118.08% and the standard deviations of all experiments were within 10%.

Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Development of an Official Analytical Method for Determination of Imazapyr in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Joo, Yoon Ji;Kim, Jinhong;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.5-13
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    • 2015
  • A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

Method Development for Determination of Multi-Mycotoxins in Chicken Liver and Kidney Tissues by LC-MS/MS (LC-MS/MS를 이용한 닭 간과 신장 중 곰팡이 독소 6종 동시분석법 개발)

  • Kim, Soohee;Kim, Kwang-Nam;Kim, Hyobi;Song, Jae-Young;Park, Sung-Won
    • Korean Journal of Poultry Science
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    • v.43 no.2
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    • pp.111-118
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    • 2016
  • Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

Quality of Life after Esophageal Surgery for Esophageal Surgery (식도암 환자의 수술 후 삶의 질에 관한 연구)

  • Kim Chong-Wook;Moon Hye-Won;Kim Yong-Hee;Park Seung-Il
    • Journal of Chest Surgery
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    • v.39 no.4 s.261
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    • pp.310-316
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    • 2006
  • Background: We study the QOL (quality of life) & functional improvement in patients underwent esophageal surgery for cancer by the viewpoint of the patient and would like make the guideline of recovery course. Material and Method: Between Dec. 1996$\sim$Aug. 2002, 250 patients were operated and 57 patients was enable interview, didn't have evidence of recurrence & survived more than 1 year postoperatively at Asan Medical Center. Questionnaire made by direct or telephone interview & include diet habitus, change of body weight, G-E (gastroesophageal) reflux, dumping symptom, change of daily life. Result: There were 53 men (93%), 4 women (7%) with mean age of $62.05{\pm}8.7$ (range: $37{\sim}94$). Operation method was Ivor Lewis operation in 43 case (75.4%), Esophagocolojejunostomy 4 case (7.1%), Mckeown operation 10 case (17.5%). In Diet habitus, 55 patients (96.5%) ate more than three times in a day with mean diet frequency was 3.5 times/day, 51 patients (89.5%) have been ate solid, regular diet, 5 patients (8.8%) enable to eat liquid diet. To compare with preoperative state, 32 patients (56.9%) had a diet speed more than 80%, 28 patients (39.1%) had a diet amount more than 80%. 32 patients (56.9%) had a little change of body weight within a 10%, 25 patients (43%) had a improvement rather than preoperative state. In G-E reflux, 4 patients (7%) had a reflux after every diet, 27 patients (47.4%) had a little reflux after diet. In dumping symptom. 7 patients (12.3%) had a diarrhea after meal. 38 patients (66.6%) had a normal activity 19 patients (33.3%) had a decreased activity. At present state, majority (53 patient-93%) of patient were satisfactory to the operation result, in spite of discomfort from time to time. In the emotional status, 50 patients (88%) had a well sleeping without disturbance. 65% of patients were comfortable in the psychology state. 39% of patients had a libido. Compare with their median age (63 y), it's a normal varient. Conclusion: QOL in patients underwent esophageal surgery for esophageal cancer nearly recovery to preoperative state.

A Study on Optimization of Nitric Acid Leaching and Roasting Process for Selective Lithium Leaching of Spent Batreries Cell Powder (폐 배터리 셀 분말의 선택적 리튬 침출을 위한 질산염화 공정 최적화 연구)

  • Jung, Yeon Jae;Park, Sung Cheol;Kim, Yong Hwan;Yoo, Bong Young;Lee, Man Seung;Son, Seong Ho
    • Resources Recycling
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    • v.30 no.6
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    • pp.43-52
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    • 2021
  • In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNixCoyMnzO2, LiCoO2) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L16(44) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO3 from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.

Improvement of an Analytical Method for Fluoroimide Residue in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Fluoroimide의 잔류농약 분석법 개선)

  • Kim, Nam Young;Park, Eun-Ji;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.220-227
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    • 2021
  • Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO4 and NaCl were used with acetonitrile. C18 (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

Determination of Residue Levels of Ethyl Carbamate in Alcoholic Beverages by Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS) (가스크로마토그래피/질량분석기(GC/MS/MS)를 이용한 주류 중 에틸카바메이트 잔류량 조사)

  • Kim, Dong-Ho;Jang, Han-Sub;Choi, Gu-Il;Kim, Hyun-Jung;Kim, Ho-Jin;Kim, Hyo-Lin;Kim, Keun-Sung
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.63-68
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    • 2013
  • Ethyl carbamate (EC) is a contaminant generated in the fermentation processes of various fermented foods. In this study, residue levels of EC in 95 alcoholic beverage samples were determined by using Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS). All the samples were purified by a liquid-liquid extraction (LLE) method using dichloromethane. The LLE method enables an improvement in time and cost to detection and specificity over the conventional extraction methods. The limits of detection and quantification (LOD and LOQ) to analyze EC were 1.3 and 4.0 ng/mL, respectively. The recovery rates of EC were ranged from 90.0 to 97.5% at the levels of 50, 100, and 500 ug/L. Among traditional grain-based alcoholic beverage samples (n = 34), the average residue levels of EC in takju, yakju, and cheongju were 0.63, 7.01, and 14.11 ug/L, respectively. Among fruit-based alcoholic beverage samples (n = 48), those of EC in japanese apricot spirits, bokbunjaju, grape wines, and other fruit wines were 79.18, 1.66, 2.64, and 2.39 ug/L, respectively. Among distilled or diluted alcoholic beverage samples (n = 13), those of EC in soju (distilled or diluted), general distillates, liquors, and brandies were 0, 3.30, 8.20, and 8.52 ug/L, respectively. Therefore, this study reports that the residue levels of EC in the alcoholic beverages, distributed in the current domestic markets, did not reach its maximum allowed levels of 30 and 400 ug/L established for grape and fruit wines in Canada, respectively.