• Title/Summary/Keyword: Sample preparation method

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Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

An Operations Study on a Home Health Nursing Demonstration Program for the Patients Discharged with Chronic Residual Health Care Problems (추후관리가 필요한 만성질환 퇴원환자 가정간호 시범사업 운영 연구)

  • 홍여신;이은옥;이소우;김매자;홍경자;서문자;이영자;박정호;송미순
    • Journal of Korean Academy of Nursing
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    • v.20 no.2
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    • pp.227-248
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    • 1990
  • The study was conceived in relation to a concern over the growing gap between the needs of chronic patients and the availability of care from the current health care system in Korea. Patients with agonizing chronic pain, discomfort, despair and disability are left with helplessly unprepared families with little help from the acute care oriented health care system after discharge from hospital. There is a great need for the development of an alternative means of quality care that is economically feasible and culturally adaptible to our society. Thus, the study was designed to demonstrate the effectiveness of home heath care as an alternative to bridge the existing gap between the patients' needs and the current practice of health care. The study specifically purports to test the effects of home care on health expenditure, readmission, job retention, compliance to health care regime, general conditions, complications, and self-care knowledge and practices. The study was guided by the operations research method advocated by the Primary Health Care Operations Research Institute(PRICOR) which constitutes 3 stages of research : namely, problem analysis solution development, and solution validation. The first step in the operations research was field preparation to develop the necessary consensus and cooperation. This was done through the formation of a consulting body at the hospital and a steering committee among the researchers. For the stage of problem analysis, the Annual Report of Seoul National University Hospital and the patients records for last 5 years were reviewed and selective patient interviews were conducted to find out the magnitude of chronic health problems and areas of unmect health care needs to finally decide on the kinds of health problems to study. On the basis of problem analysis, the solution development stage was devoted to home care program development asa solution alternative. Assessment tools, teaching guidelines and care protocols were developed and tested for their validity. The final stage was the stage of experimentation and evaluation. Patients with liver diseases, hemiplegic and diabetic conditions were selected as study samples. Discharge evaluation, follow up home care, measurement and evaluation were carried out according to the protocols of care and measurement plan for each patient for the period of 6 months after discharge. The study was carried out for the period from Jan. 1987 to Dec. 1989. The following are the results of the study presented according to the hypotheses set forth for the study ; 1. Total expenditures for the period of study were not reduced for the experimental group, however, since the cost per hospital visit is about 4 times as great as the cost per home visit, the effect of cost saving by home care will become a reality as home care replaces part of the hospital visits. 2. The effect on the rate of readmission and job retention was found to be statistically nonsignificant though the number of readmission was less among the experimental group receiving home care. 3. The effect on compliance to the health care regime was found to be statistically significant at the 5% level for hepatopathic and diabetic patients. 4. Education on diet, rest and excise, and medication through home care had an effect on improved liver function test scores, prevention of complications and self - care knowledge in hepatopathic patients at a statistically significant level. 5. In hemiplegic patient, home care had an effect on increased grasping power at a significant level. However. there was no significant difference between the experimental and control groups in the level of compliane, prevention of complications or in self-care practices. 6. In diabetic patients, there was no difference between the experimental and control groups in scores of laboratory tests, appearance of complications, and self-care knowledge or self -care practices. The above findings indicate that a home care program instituted for such short term as 6 months period could not totally demonstrate its effectiveness at a statistically significant level by quantitative analysis however, what was shown in part in this analysis, and in the continuous consultation sought by those who had been in the experimental group, is that home health care has a great potential in retarding or preventing pathological progress, facilitating rehabilitative and productive life, and improving quality of life by adding comfort, confidence and strength to patients and their families. For the further studies of this kind with chronic patients it is recommended that a sample of newly diagnosed patients be followed up for a longer period of time with more frequent observations to demonstrate a more dear- cut picture of the effectiveness of home care.

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Identification of Microplastics in Sea Salts by Raman Microscopy and FT-IR Microscopy (라만 및 FT-IR 현미경을 이용한 천일염 중 미세플라스틱 분석)

  • Cho, Soo-Ah;Cho, Won-Bo;Kim, Su-Bin;Chung, Jae-Hak;Kim, Hyo-Jin
    • Analytical Science and Technology
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    • v.32 no.6
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    • pp.243-251
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    • 2019
  • Microplastics (MP) are found in large quantities in the oceans, posing a major threat to the ecosystem. In Korea, MPs have been reported to be detected in sea salts. In order to analyze MPs, information on their composition, size, and shape is required. FT-IR microscopy is used frequently to measure sizes larger than 20 ㎛. Recently, however, Raman microscopy, which can analyze ultrafine plastics below 20 ㎛, has been applied extensively. In this study, 10.0 g samples of commercially available salts were dissolved and filtered through a 45 ㎛ mesh filter with a size of 25.4 mm × 25.4 mm. These filtered samples were then analyzed by both FT-IR microscopy and Raman microscopy. A total of four MPs, including three polyethylene (PE) of size 70-100 ㎛ and a polypropylene (PP) of size 170 ㎛, were detected by FT-IR microscopy, while 10 MPs, including nine PE of size 10-120 ㎛ and one polystyrene (PS) of size 40 ㎛, were detected by Raman microscopy. Approximately, 1,000 MPs/kg was estimated, which was almost two times higher than the previous reported levels (~550-681 particles/kg in sea salts); this is because Raman microscopy can detect much smaller MPs than FT-IR microscopy. A total of 113 particles were found using Raman microscopy: Carbon (35, 31.5 %), minerals (28, 25 %), and glass (16, 14.4 %) were dominant, forming around 70% of the total, but MPs (10, 8.8 %) and cellulose (5, 4.5 %) were also found. Raman microscopy has great potential as an accurate method for measuring MPs, as it can measure smaller size MPs than FT-IR microscopy. It also has a reduced sample preparation time.

tans-Resveratrol Content of Varieties and Growth Period in Peanut (땅콩 품종 및 생육기별 trans-Resveratrol 함량)

  • Lee, Mi-Ja;Cheong, Young-Keun;Kim, Hyung-Soon;Park, Ki-Hun;Doo, Hong-Soo;Suh, Duck-Yong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.48 no.6
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    • pp.429-433
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    • 2003
  • trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

Identification and Fermentation Characteristics of Lactic Acid Bacteria Isolated from Dongchimi as Starter for Radish Juice (무 쥬스 제조를 위한 starter로써 동치미에서 분리한 유산균의 동정 및 발효 특성)

  • Kim, Jung-Hee;Kim, Jong-Il
    • Korean Journal of Microbiology
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    • v.35 no.4
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    • pp.307-314
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    • 1999
  • This study was aimed at the investigation of the possibility of the addition of lactic acid bacteria as "starter"for the preparation of radish juice. Forty strains of lactic acid bacteria were isolated from dongchimi that was fermented by a traditional method. The isolates were assorted into 5groups, Leuconostoc mesenteroides subsp. mesenteroides (J-9), Lacobacillus brevis (J-12), Lactobacillus fermentum (J-7), Lactobacillus sake (J-20), and Lactobacillus plantarum (J-39). Leuconostoc mesenteroides was predominated in the sample of dongchimi with frequency of 52.5%. Each of the strain, which exhibited the beat growth in the species, was selected in the 5species, and investigation of the fermentation characteristcis was carried out. The fermentation were performed for 9 days at 25${\circ}C$ after the inoculation of 0.3% ($10^{6}$ cfu/㎖) to each ultra-filtrated radish juice. The pH, total acidity, content of non-volatile organic acids were examined during the fermentation period. Lactobacillus plantarum showed the highest growth rate and the growth rate of Lactobacillus sake was the lowest. The pH (6.3-6.36) and total acidity (0.09-1.0 %) fo the ultrafiltrated radish juice before fermentation were changed to 3.2-4.3 and 0.65-1.2% after 9days, respectively. The changes of the pH and total acidity were related with the growth of the lactic acid bacteria; the better growth of lactic acid bacteria, the more rapid decrease of pH and increase of the total acidity. when the amount of non-volatile organic acids were estimated during fermentation, citric acid, malic acid, malonic acid, and succinic acid were decreased in all cases. However, the content of lactic acid increased with the progression of fermentation. L. mesenteroides (J-9), L. brevis (J-12) and L. fermentum (J-7) were chosen for the candidates of the starter for the lactic fermentation of radish juice based on the biochemical analysis and sensory evaluation.

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Quality Characteristics and Antioxidant Properties of Saccharified Banana Gruels (바나나 첨가량을 달리한 당화 바나나죽의 품질특성 및 항산화효과)

  • Kim, Jin Sook;Kim, Ja Young;Kim, Gi Chang;Kim, Kyung Mi;Kang, Myung Hwa
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.7
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    • pp.1071-1078
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    • 2013
  • We conducted this study in order to investigate the quality and antioxidant properties of saccharifed banana gruel containing different levels (0, 15, 30, and 45%) of banana puree. Saccharified banana gruel with different ratios of banana was prepared and proximate composition, sweetness ($^{\circ}brix%$), pH, total acidity, Hunter's color value, viscosity, free sugar, sensory evaluation, and physiological activities of the sample were measured. With increasing banana content, proximate composition, sweetness, and acidity of banana gruel increased, and pH showed a significant decrease (P<0.05). Saccharified banana gruel prepared with 15~45% banana showed significantly lower viscosity. As the level of banana increased, L-value decreased, whereas the a-value, b-value increased. Free sugar content of fructose, glucose, maltose, and sucrose showed a significant increase (P<0.05). Saccharified banana gruel with 30% added banana was the most preferred for color, flavor, taste, mouth-feeling, texture, and overall acceptability. The total phenolic compound contents of saccharified banana gruel with banana puree ranged from 1.73 to 5.75 mg/g. DPPH and ABTS radical scavenging activities of saccharified banana gruel with banana puree were 8.67~31.26% and 6.02~55.16%, respectively. With increasing banana content, total polyphenol contents, DPPH and ABTS radical scavenging activity of banana gruel showed a significant increase (P<0.05). From these results, we found that addition of 30% banana was the best method for preparation of gruel with high sensory quality.

Preparation of Pure CO2 Standard Gas from Calcium Carbonate for Stable Isotope Analysis (탄산칼슘을 이용한 이산화탄소 안정동위원소 표준시료 제작에 대한 연구)

  • Park, Mi-Kyung;Park, Sunyoung;Kang, Dong-Jin;Li, Shanlan;Kim, Jae-Yeon;Jo, Chun Ok;Kim, Jooil;Kim, Kyung-Ryul
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.18 no.1
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    • pp.40-46
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    • 2013
  • The isotope ratios of $^{13}C/^{12}C$ and $^{18}O/^{16}O$ for a sample in a mass spectrometer are measured relative to those of a pure $CO_2$ reference gas (i.e., laboratory working standard). Thus, the calibration of a laboratory working standard gas to the international isotope scales (Pee Dee Belemnite (PDB) for ${\delta}^{13}C$ and Vienna Standard Mean Ocean Water (V-SMOW) for ${\delta}^{18}O$) is essential for comparisons between data sets obtained by other groups on other mass spectrometers. However, one often finds difficulties in getting well-calibrated standard gases, because of their production time and high price. Additional difficulty is that fractionation processes can occur inside the gas cylinder most likely due to pressure drop in long-term use. Therefore, studies on laboratory production of pure $CO_2$ isotope standard gas from stable solid calcium carbonate standard materials, have been performed. For this study, we propose a method to extract pure $CO_2$ gas without isotope fractionation from a solid calcium carbonate material. The method is similar to that suggested by Coplen et al., (1983), but is better optimized particularly to make a large amount of pure $CO_2$ gas from calcium carbonate material. The $CaCO_3$ releases $CO_2$ in reaction with 100% pure phosphoric acid at $25^{\circ}C$ in a custom designed, evacuated reaction vessel. Here we introduce optimal procedure, reaction conditions, and samples/reactants size for calcium carbonate-phosphoric acid reaction and also provide the details for extracting, purifying and collecting $CO_2$ gas out of the reaction vessel. The measurements for ${\delta}^{18}O$ and ${\delta}^{13}C$ of $CO_2$ were performed at Seoul National University using a stable isotope ratio mass spectrometer (VG Isotech, SIRA Series II) operated in dual-inlet mode. The entire analysis precisions for ${\delta}^{18}O$ and ${\delta}^{13}C$ were evaluated based on the standard deviations of multiple measurements on 15 separate samples of purified $CO_2$. The pure $CO_2$ samples were taken from 100-mg aliquots of a solid calcium carbonate (Solenhofen-ori $CaCO_3$) during 8-day experimental period. The multiple measurements yielded the $1{\sigma}$ precisions of ${\pm}0.01$‰ for ${\delta}^{13}C$ and ${\pm}0.05$‰ for ${\delta}^{18}O$, comparable to the internal instrumental precisions of SIRA. Therefore, we conclude the method proposed in this study can serve as a way to produce an accurate secondary and/or laboratory $CO_2$ standard gas. We hope this study helps resolve difficulties in placing a laboratory working standard onto the international isotope scales and does make accurate comparisons with other data sets from other groups.