• Title/Summary/Keyword: 검출기 감도

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Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

Study on establishment of emission cell test method for liquid phase building materials (방출셀을 이용한 액상건축자재 오염물질 방출시험방법 정립에 관한 연구)

  • Lim, Jungyun;Jang, Seongki;Seo, Sooyun
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.191-200
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    • 2009
  • The aim of this study was to evaluate and establish of emission test method for liquid phase building materials such as paint, adhesive, sealant by emission cell. A small-scale emission chamber and emission cell were used to evaluate emission of TVOC from paint, adhesive, sealant. The quantity of TVOC emission were measured by a gas chromatography/mass spectrometry (GC/MS). Background concentration of TVOC was below $10{\mu}g/m^3$ in the emission chamber and cell. Air tightness and recovery in chamber and cell showed good results. The recovery of thermal desorber for toluene and n-dodecane were about 120%. The repeatability of response factor and retention time in GC/MS below 30%. The method detection limit of VOCs ranged 0.04~8.82 ng. The concentration of TVOC emission using emission cell was 1.35~1.41 times higher than emission chamber. The correlation of TVOC emission using chamber and cell method was significantly high (r=0.91~0.97).

된장절임기간에 따른 새송이버섯의 품질 변화 특성

  • 황성희;이예경;윤광섭;김순동
    • Proceedings of the Korean Society of Postharvest Science and Technology of Agricultural Products Conference
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    • 2003.04a
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    • pp.117.2-118
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    • 2003
  • 절임식품은 우리 고유의 먹거리이지만 체계적인 연구가 부족하여 품질표준화가 이루어지지 않고 있어 우리의 전통식품을 세계적인 식품으로 개발하기 위해서는 전통식품을 과학화하고 현대화할 수 있는 연구가 필요하다. 새로운 된장절임 가공법을 개발하고자 blanching, salting, drying 등의 전 처리를 행한 후 된장 절임기간에 따른 새송이 버섯의 수분함량, 염도, 색상, 조직특성, 관능특성 등의 변화를 조사하였다. 된장절임기간에 따른 새송이 버섯의 수분함량 변화는 숙성시간이 경과함에 따라 감소하였으며 염도는 시간이 지남에 따라 증가하는 경향을 보였으나 무처구를 제외하고는 숙성 30일 이후부터는 변화가 거의 없었다. 숙성기간에 따른 색상의 변화를 보면 블랜칭이 매우 효과적으로 변색을 방지하였다. 숙성 30일부터는 모든 처리구에서 강도가 저하하는 경향을 보였으며 관능평가 결과 숙성 40일째에 맛과 조직감 그리고 기호도 등 모든 항목에서 B(B)와 E(BSD) 처리구가 높은 점수를 받아 관능적 품질 특성이 가장 우수하였다. 이상의 결과로 볼 때 전처리공정에 있어서는 7$0^{\circ}C$에서 10분간 블랜칭처리한 B(B)처리구가 가장 우수하였으나 된장 절임후 숙성기간이 경과함에 따라서는 7$0^{\circ}C$에서 10분간 블랜칭처리후 5% 염용액에서 72시간 절임한 후 4$0^{\circ}C$에서 30분간 탈염하고, 다시 5$0^{\circ}C$의 온도에서 3시간 건조시킨 E(BSD)처리구도 우수한 품질을 유지할 수 있어 새송이 버섯을 이용한 장류절임가공법으로 활용이 가능함을 확인하였다.d, citric acid 그리고 shikimic acid가 검출되었고 수확시기에 3품종에서 모두 malic acid 함량이 가장 높았고 malic acid와 citric acid의 함량이 풍수와 신고에서는 약 0.3%, 추황은 0.4% 이상으로 나타났다. 또한 3품종 모두에서 총산과 같은 추세로 성숙기의 유기산의 함량이 생장초기의 함량보다 많이 감소되었음을 알 수 있었다. 배의 가용성 고형물은 전체적으로 과실의 성장이 진행됨에 따라 증가하는 추세를 나타내었다. 풍수와 신고 과피의 총당과 환원당은 거의 같은 추세로 증가하였고 성숙이 가까워지면서 환원당이 감소하였다. 배 과육의 총당과 환원당 또한 거의 같은 추세로 증가를 하다가 수확 전 20일 혹은 30일부터 총당의 함량은 계속 증가하지만 환원당의 함량은 큰 변화가 없는 것으로 나타났다. 배 과실의 전반 성장과정에 있어서 전분함량은 감소하였고 총탄수화물의 함량은 과육에서는 증가하나 과피에서는 반대로 감소하는 경향을 보였다. 풍수의 전분함량은 최고 2.19%에서 0.23%로 감소하였고 신고에서는 0.43%로 추황에서는 0.48%로 감소하였다. 배 유리당은 fructose, glucose, sorbitol, sucrose 둥 4종류의 당이 검출되었고 3품종 모두에서 생장과정 중 비환원당인 sucrose 함량은 계속 증가하였고 fructose, glucose, sorbitol의 함량(추황의 sorbitol을 제외)은 생장이 촉진됨에 따라 증가하다가 다시 점차적으로 감소하였다. 이러한 결과는 총당과 환원당의 측정결과와 일치한 것으로 나타났다. 결론적으로 배의 성장에 따라 산 함량은 감소하였고 당 함량은 증가하였다.luco-pyranosi

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Preconcentration and Determination of Trace Cobalt and Nickel by the Adsorption of Metal-PDC Complexes on the Anion-Exchange Resin Suspension (금속-PDC 착물의 음이온교환 수지 상 흡착에 의한 흔적량 코발트와 니켈의 동시 예비농축 및 정량)

  • Han, Chul-Woo;In, Gyo;Choi, Jong-Moon;Kim, Sun Tae;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.608-615
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    • 2000
  • A determination method of trace nickel and cobalt in water samples was studied and developed by adsorbing their complexes on ion exchange resin suspension. The analytical ions were formed as complexes with a ligand of APDC (ammonium pyrrolidinedithiocarbamate) and adsorbed on anion exchange resin of Dowex 2-X8. After the suspension was filtered out with membrane filter, the complexes were dissolved in HCl solution by an ultrasonic vibrator for ET-AAS determination. Several conditions were optimized as followings. pH of sample solution: 5.0, amount of ligand APDC: more than 430 times in mole ratio, the type and concentration of acid: 0.1 M HCl, and vibration time: 7 minutes. The addition of palladium in the HCl solution could improve the reproducibility and sensitivity by a matrix modification in the absorbance measurement. This procedure was applied for the analysis of three kinds of real water samples. The detection limits equivalent to 3 times standard deviation of blank were Co 0.36 ng/mL and Ni 0.27 ng/mL and recoveries in spiked samples were 99-102% for cobalt and 100-105% for nickel.

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Assessment of Natural Radiation Exposure by Means of Gamma-Ray Spectrometry and Thermoluminescence Dosimetry (감마선분광분석(線分光分析) 및 열형광검출법(熱螢光檢出法)에 의한 자연방사선(自然放射線)의 선량측정연구(線量測定硏究))

  • Jun, Jae-Shik;Oh, Hi-Peel;Choi, Chul-Kyu;Oh, Heon-Jin;Ha, Chung-Woo
    • Journal of Radiation Protection and Research
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    • v.10 no.2
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    • pp.96-108
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    • 1985
  • A study for the assessment of natural environmental radiation exposure at a flat and open field of about $10,000m^2$ in area in CNU Daeduk campus has been carried out by means of gamma-ray scintillation spectrometry and thermoluminescence dosimetry for one year period of time from October 1984. The detectors used were 3'${\phi}{\times}$3' NaI(T1) and two different types of LiF TLD, namely, chip sealed in plastic sheet which tightly pressed on two open holes of a metal plate and Teflon disk. Three 24-hour cycles of in-situ spectrometry, and two 3-month and one 1-month cycles of field TL dosimetry were performed. All the spectra measured were converted into exposure rate by means of G(E) opertaion, and therefrom exposure rate due to terrestrial component of environmental radiation was figured out. Exposure rate determined by the spectrometry was, on average, $(10.54{\pm}2.96){\mu}R/hr$, and the rates of $(12.0{\pm}3.4){\mu}R/hr$ and $(11.0{\pm}3.6){\mu}R/hr$ were obtained from chip and disk TLD, respectively. Fluctuations in diurnal variation of the exposure rate measured by the spectrometry were noticeable sometime even in a single cycle of 24 hours. It is concluded that appropriately combined use of TLD with iu-sitn gamma-ray spectrometry system can give more accurate and precise measure of environmental radiation exposure, and further study for more adequate and sensitive TLD for environmental dosimetry, including improvement and elevation of accuracy in data assessment through inter-laboratory or international intercomparison is necessary.

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Quality Characteristics of Kimchi according to Garlic Content during Fermentation (마늘 첨가량에 따른 김치의 발효 중 품질 특성 변화)

  • Choi, Yun-Jeong;Hwang, Ye-Seul;Hong, Sung Wook;Lee, Mi-Ai
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.11
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    • pp.1638-1648
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    • 2016
  • This study was conducted to analyze the quality characteristics of kimchi in terms of garlic content (0~4.5%). Kimchi was made at $4^{\circ}C$ for 8 weeks, and pH, acidity, organic acid content, free sugar content, microbial counts, flavor pattern, and sensory characteristics were measured. The results show that kimchi containing garlic had a higher pH and lower acidity during fermentation than control kimchi without garlic. Principal component analysis enabled differentiation of the flavor pattern of kimchi according to fermentation period and garlic content. Addition of garlic to kimchi significantly decreased the numbers of total bacteria and lactic acid bacteria for 2 weeks after production. The numbers of total bacteria and lactic acid bacteria increased rapidly up to 2 weeks during fermentation and thereafter decreased gradually. Coliform counts were higher in the control than in kimchi containing garlic, whereas there was no detection after 4 weeks. Yeast and mold counts decreased significantly with increasing garlic content during the initial fermentation stage. Counts could not be detected in kimchi containing garlic. After 4 weeks, counts could not be detected in kimchi without garlic. Among kimchi with different garlic contents, fermentation was slower in kimchi with high garlic content; scores for off-odor and off-note taste were lower as well.

Development of Rapid Analysis Method for Pesticide Residues by GC-MS/MS (GC-MS/MS를 이용한 잔류농약 신속검사법 개발)

  • Choi, Yong-Hoon;Nam, Hye-Seon;Hong, Hye-Mi;Lee, Jin-Ha;Chae, Kab-Ryong;Lee, Jong-Ok;Kim, Hee-Yun;Yoon, Sang-Hyeon
    • The Korean Journal of Pesticide Science
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    • v.9 no.4
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    • pp.292-302
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    • 2005
  • Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.

Determination of Soluble Carbohydrates in Soybean Seeds Using High Performance Liquid Chromatography with Evaporative Light Scattering Detection (증기화광산란 검출기를 이용한 콩 함유 수용성 탄수화물의 분석)

  • Kim, Gyeong-Ha;Hwang, Young-Sun;Ahn, Kyung-Geun;Kim, Gi-Ppeum;Kim, Min-Ji;Hong, Seung-Beom;Moon, Jung-Kyeong;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.7
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    • pp.1062-1067
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    • 2014
  • In the present study, a new analytical method was devised for the simultaneous determination of soluble carbohydrates in soybean seeds using high performance liquid chromatography/evaporative light scattering detection (HPLC/ELSD). The limit of quantification (LOQ) for soybean soluble carbohydrates ranged from 5.6~7.6 mg/kg using the HPLC/ELSD method and from 16.2~33.9 mg/kg using the high performance liquid chromatography/refractive index detection (HPLC/RID) method. Therefore, the HPLC/ELSD method was more sensitive than HPLC/RID. The precision values for retention time and peak area of the HPLC/ELSD method were evaluated by inter-day (n=5) and intra-day (n=10) assays using a standard solution. All precision values (CV<2.5%) for soybean soluble carbohydrates were acceptable and fulfilled international acceptance criteria. All linear calibration curves were obtained with a correlation coefficient of $R^2$ >0.999. The contents of soluble carbohydrates for the "Shingikong" (yellow soybean) and "Cheongjakong 3" (black soybean) samples were analyzed using the HPLC/RID and HPLC/ELSD methods. The difference in carbohydrate contents between the two detection methods was significant. Carbohydrate contents in the HPLC/ELSD method were higher than those in the HPLC/RID method. Overall, the HPLC/ELSD method showed satisfactory resolution with a favorable LOQ and reproducibility. Therefore, these results indicate that the HPLC/ELSD method may be applied to determine the contents of soluble carbohydrates in soybean seeds and related food stuffs.

Use of Auxins for Rhizome Propagation and Shading Effect on Growth of Asarum sieboldii Mio. (세신(細辛)의 근경삽(根莖揷)번식에 있어서 오옥신의 이용과 차광재배(遮光栽培))

  • Kim, Sun-Gon;Park, Chung-Heon;Choi, Dong-Geun;Hwang, Chang-Ju;Chin, Seong-Kye
    • Korean Journal of Medicinal Crop Science
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    • v.2 no.3
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    • pp.198-204
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    • 1994
  • This study was carried out to investigate the auxin(IAA, IBA, NAA) treatment and the effect of shading rate in Asarum sieboldii. The results obtained were summerized as follows: By the soaking treatment of auxins to the cutted rhizome enhanced root growth and plant weight. By the increment of shading rate, plant growth was much better compare to the control. Leaf fallen times appeared about 20 days more earlier at plain area then the alpain area. Root yield was much higher by the treatment of shading then the conventional cultivation so it seem to be the useful for large scale cultivations of A. sieboldii.

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Investigation on the Management of Livestock Wastes and VOCs Concentration of Farms in Daejeon Area (대전광역시 양축농가의 축분뇨 관리 실태 및 VOCs 농도 조사)

  • Lee, Bong-Duk;Lee, Soo-Kee;Oh, Hong-Rok;Heo, Jung-Min;Jung, Kie-Chul;Kim, Sung-Bok
    • Korean Journal of Agricultural Science
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    • v.32 no.1
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    • pp.43-51
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    • 2005
  • This study was carried out to investigate the style of livestock house, concentration of malodorous substances of livestock feces and livestock houses in Daejeon area. Among the livestock houses investigated, as most of cow pens(94.5%) have sawdust or chaff on the bottom, there was no leakage of feces out of pen. Most pig pens adopted slury style, but some of them currently use buffering material on the bottom. It is thought that there will be no possible contamination leakage. When it comes to hen house, all the broiler house use litters on the bottom and all the layer house use scrapper. It is also thought that there will be no possible contamination leakage. 3 out of 12 deer pens used buffering material on the bottom, 10 places were maintained in a traditional method, and 7 places left possibility of contamination leakage considering whether the roof was installed or not. The contents of ammonia, amine and volatile fatty acid in fresh feces were lower compared to rotten feces, but the concentration of sulfur-containing matter - hydrogen sulfide, methylmercapthan and ethylmercapthan were higher compared to rotten feces. In the case of malodorous ingredient in livestock houses, only small amount of ammonia and hydrogen sulfide were detected in pig pen and hen house, and other ingredients were not detectable. And those who are engaged in animal husbandry reacted negatively to the use of feed additives for decreasing malodor. In conclusion, it is not worrisome that contamination can be leaked out of animal raising facilities. But if we take into consideration that the point of investigation time is wintry season, there should be more considerate attitude. And feed additives for decreasing malodor need establishing criteria in the manufacturing process.

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