• Title/Summary/Keyword: Instrumental analyses

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PREDICTION OF PHYSICO-CHEMICAL AND TEXTURE CHARACTERISTICS OF BEEF BY NEAR INFRARED TRANSMITTANCE SPECTROSCOPY

  • Olivan, Mamen;Delaroza, Begona;Mocha, Mercedes;Martinez, Maria Jesus
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1256-1256
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    • 2001
  • The physico-chemical and texture characteristics of meat determine the nutritional, technological and sensory quality. However, the analysis of meat quality requires expensive, laborious and time consuming analytical methods. The objective of this study was to evaluate NIR spectroscopy using transmittance for determining the moisture, fat, protein and total pigment content, the water holding capacity (WHC) and the toughness of beef meat. A total of 318 spectra were recorded from ground beef samples by a Feed Analyzer 1265 of Infratec. The samples were obtained from the Longissimus muscle of the 10$^{th}$ rib of yearling bulls, ground with an electrical chopper, vacuum packaged, aged during 7 days and frozen at -24$^{\circ}C$ until the analyses were done. Moisture content was measured by oven drying at 10$0^{\circ}C$, fat content was determined by Soxhlet extraction and protein content was estimated from nitrogen content using the Kjeldahl analysis. The total pigment content was determined by the method of Hornsey and the WHC using the method of filter paper press. The instrumental evaluation of texture (maximum load WB, maximum stress MS and toughness) was conducted in an Instron equipment with a Warner-Bratzler shearing device. This analysis was performed on a chop of 3.5 cm obtained from the longissimus of the 8$^{th}$ rib, aged during 7 days, kept frozen at -24$^{\circ}C$ and cooked before the analysis. Near infrared spectra were recorded as log 1/T (T=transmittance) at 2 nm intervals from 850 to 1050 nm using a Feed Analyzer 1265 of Infratec. Calibrations were performed with the WinISI software (vs. 1.02) using the MPLS method. To examine the effect of scatter correction o. derivation of spectra on the calibration performance, calibrations were calculated with the crude spectra or pretreated with different mathematical treatments (inverse MSC, SNVD) and/or second derivative operation. For chemical composition, the use of the scatter corrections improved the calibration statistics, in terms of lower SECV and higher $r^2$. In most of the variables, the use of the 2$^{nd}$ derivative improved the predictions, mainly when combined with the SNVD treatment. However, for predicting the texture traits, the best estimation was obtained from the crude spectrum. These results showed that the equations obtained for predicting moisture, fat and total pigments were very accurate, with $r^2$ being higher that 0.9. However, the prediction of the texture traits (WB, MS, toughness) from ground meat was poor.

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Effects of Methacrylamide Treatment on Silk Fibers III. Polymerization Behavior of Methacrylamide (견섬유에 대한 메타크릴아미드의 처리효과 III. 메타크릴아미드의 중합거동)

  • 신봉섭;남중희
    • Journal of Sericultural and Entomological Science
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    • v.34 no.2
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    • pp.32-40
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    • 1992
  • Many studies have been carried out on the graft finishing in order to improve the quality of silk fiber. Various vinyl monomers, for instance, styrene, methylmethacrylate, 2-hydroxyeth-ylmethacrylate and methacrylamide, have been used practically up to date. Among these monomers, methacrylamide has been applied as the most favourable monomer onto silk fibers in recent years. The polymerization mechanism about styrene- and methylmethacrylate-grafted silk fiber has been studied by many researchers. They proposed that free radicals were formed and vinyl monomers were polymerized in silk fibroin by graft polymerization mechanism, while active sites were varied by the types of monomer and initiator as well as by the reaction condition. In general. there is another Opinion that monomers are polymerized and impregnated in the internal side of the fiber by homopolymerization, which has not been proved experimentally yet More than 10 years have been passed since methacrylamide was applied on the silk fiber, and at the present time most finishings are being achieved by methacrylamide. However, no attention has been paid to the polymerization mechanism of the methacrylamide-treated silk fiber yeL In this paper, the treatments of methacrylamide on silk fibers were studied in aqueous solution using potassium persulfate as an initiator. The polymerization mechanism of the methacrylamide-treated silk fibers was investigated and analyzed on the basis of the results of infrared spectroscopy, amino acid analysis and scanning electron microscopy. From the results of these instrumental analyses, it can be suggested that polymerization mechanism about the methacrylamide-treated silk fibers is not performed by graft polymerization which has been accepted generally in styrene and methylmethacrylate-grafted silk fibers. The different mechanism is supposed to be due to the difference in monomer types, initiator types and treatment conditions.

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The Health and Dietary management of Impaired elderly by ADL in Gyeonggi, Korea (ADL에 의한 도움필요 노인의 건강과 식생활관리 -경기지역 농촌노인을 중심으로-)

  • Rhie Seung-Gyo;Choi Mi-Yong;Won Hyang-Rye
    • The Korean Journal of Community Living Science
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    • v.17 no.3
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    • pp.159-174
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    • 2006
  • The purpose of this study is to provide information searching for health promotion, nutrition improvement, and health care of the impaired elderly by ADL(Activity of Daily Living) and IADL(Instrumental Activity of Daily Living). The subjects were divided into the Assistant Needed Group and No Assistant Needed Group for living in line with the responses of ADL(10 items like dressing, washing, move etc.) and IADL(10 items like housekeeping, using transportation, shopping, Phone call etc.). Survey was made for health behavior, health risk habit, dietary management status and diet intake by 24 hr-recall and questionnaire method. 242 subjects were collected in 12 cities or Gun districts in Gyeonggi Province, S. Korea. Survey was carried out by regional home extension workers using interview method. Statistical analyses were made using SAS (Version 8.1). Chi-Square Tests and General Linear Models. The subjects of impaired ADL elderly was 26.5% and it composed 30% of the total male and 22.2% of the total female. The demographic status of the impaired ADL elderly showed no difference from that of the normal elders, elementary school educated (73.4%), with spouse (43.8%) or with adult children(37.5%), using monthly living cost of 500-1,000 thousand won(35.9%). Mean age was 74.05 years compared to 72.25 years of normal elders. However, there was no significant difference from the normal and impaired ADL group, regular exercise(60.0%), with walking (90.0%), no-smoke(54.7%) and no-drink(48.4%). Kind of disease was not different from the one in impaired and normal group, with cardiovascular disease(32.3%), with diabetes mellitus(8.1%), joint lumbago neuralgia(32.3%) and osteoporosis(9.7%). Gastrointestinal complaints of the impaired ADL group were nausea(57.8%), chronic indigestion (23.4%), constipation (14,0%) and vomiting(3.7%). Sleeping time required for the impaired was longer than that for the normal group by 10hours(4.7%) or 8-10hours(20.3%), which consisted 1.7% and 16.6% respectively. Nutrient intake of the impaired ADL group was low compared to normal range elders: Energy(1260kca1), Protein(52.75g). There was gender difference in nutrient intake; the male impaired group showed no significant difference from the normal group but it was significantly lower in female impaired group. These results suggest that low quality of life and low economic status of the impaired ADL elderly require congregate meal in village hall to cover the lack of side dishe variety. And nutrition education program including community assistance would be required for the impaired ADL elderly together with the sufficient food and exercise practice. By operating nutrition education program, the impaired ADL elderly would maintain more enhanced quality of life and ameliorate the ADL capability.

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Case Study of the Stability of a Large Cut-Slope at a Tunnel Portal (터널 입구부 대절토 사면 안정성 사례 연구)

  • Park, Dong Soon;Bae, Jong-Soem
    • The Journal of Engineering Geology
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    • v.25 no.1
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    • pp.115-129
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    • 2015
  • The cut-slope of a large-sectional tunnel portal is recognized as a potential area of weakness due to unstable stress distribution and possible permanent displacement. This paper presents a case study of a slope failure and remediation for a large-scale cut-slope at a tunnel portal. Extensive rock-slope brittle failure occurred along discontinuities in the rock mass after 46 mm of rainfall, which caused instability of the upper part of the cut-slope. Based on a geological survey and face mapping, the reason for failure is believed to be the presence of thin clay fill in discontinuities in the weathered rock mass and consequent saturationinduced joint weakening. The granite-gneiss rock mass has a high content of alkali-feldspar, indicating a vulnerability to weathering. Immediately before the slope failure, a sharp increase in displacement rate was indicated by settlement-time histories, and this observation can contribute to the safety management criteria for slope stability. In this case study, emergency remediation was performed to prevent further hazard and to facilitate reconstruction, and counterweight fill and concrete filling of voids were successfully applied. For ultimate remediation, the grid anchor-blocks were used for slope stabilization, and additional rock bolts and grouting were applied inside the tunnel. Limit-equilibrium slope stability analysis and analyses of strereographic projections confirmed the instability of the original slope and the effectiveness of reinforcing methods. After the application of reinforcing measures, instrumental monitoring indicated that the slope and the tunnel remained stable. This case study is expected to serve as a valuable reference for similar engineering cases of large-sectional slope stability.

Prolyl Endopeptidase-inhibiting Isoflavonoids from Puerariae Flos and Some Revision of their $^{13}C-NMR$ Assignment (갈화의 Prolyl Endopeptidase 저해 활성 Isoflavonoid 및 이들의 $^{13}C-NMR$ Assignment)

  • Kim, Kyung-Bum;Kim, Sang-In;Kim, Jong-Sik;Song, Kyung-Sik
    • Applied Biological Chemistry
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    • v.42 no.4
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    • pp.351-355
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    • 1999
  • In order to find anti-dementia drugs from natural products, prolyl endopeptidase inhibitors were purified from Puerariae Flos by consecutive solvent partition, followed by silica gel, Sephadex LH-20, and HPLC. Four isoflavonoid inhibitors were isolated and identified as tectorigenin, genistein, 5,7-dihydroxy-4',6-dimethoxyisoflavone, and 5-hydroxy-6,7,4'-trimethoxyisoflavone by means of instrumental analyses including $^{1}H-$, $^{13}C-$, $^{2}D-NMR$ and MS and $IC_{50}$ values against PEP were 5.30 ppm$(17.7\;{\mu}M)$, 10.39 ppm$(38.5\;{\mu}M)$, 13.92 ppm$(44.3\;{\mu}M)$, and 20.61 ppm$(62.8\;{\mu}M)$, respectively. Some previous mistakes in $^{13}C-NMR$ assignment were revised by careful investigation of HMBC and HMQC data.

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Toxicity of the Imported Pufferfish, Fugu flavidus ('Samchaebog'), from China (중국으로부터 수입된 삼채복(Fugu flavidus)의 독성)

  • KIM Dong-Soo;KIM Sang-Rok;LEE Myung-Ja;SEOL Myung-Hoon;JEONG Dong-Youn;KIM Hyun-Dae
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.28 no.5
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    • pp.533-538
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    • 1995
  • Ten specimens of the imported pufferfish, fugu flavidus ('Sarnchaebog'), from China were assayed for anatomical distribution of toxicity, Also, a toxic ovary of each specimen was excised, and transferred into Bio-gel P-2 column chromatography for purification of the toxins. The average toxicity of all specimens assayed was calculated to be $4.1\pm 0.5\;in\;liver,\;2.8\pm1.1\;intestine,\;0.8\pm0.5\;skin,\;2.3\pm1.5\;testis\;39.0\pm16.0\;ovary\;and\;7.0\pm2.0 MU/g$ bile, respectively; Ovary was weakly toxic, but others were non-toxic or weakly toxic. Moreover, instrumental analyses including thin layer chromatography(TLC) and electrophoresis disclosed tetrodotoxin (TTX) and anhydro tetrodotoxin (anh-TTX), respectively. The toxins of the ovary gave four peaks in high performance liquid chromatography (HPLC) whose retention times (14 and 24 min) were close to those of TTX and anh-TTX, respectively.

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Preparation of Self-repairing Polymer-modified Waterproofing Asphalt-montmorillonite Composite: 2. Validation of Optimized Silylation of Montmorillonite (K-10) Using 3-aminopropyltriethoxysilane (자가치유성을 갖는 고분자개질 방수아스팔트-몬모릴로나이트 composite 제조: 2. 3-aminopropyltriethoxysilane에 의한 몬모릴로나이트(K-10)의 실란화 최적화 검증)

  • Lee, Eun Ju;Lee, Jong Hoon;Lim, Kwang-Hee
    • Korean Chemical Engineering Research
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    • v.55 no.3
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    • pp.409-418
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    • 2017
  • In preparation of self-repairing polymer-modified waterproofing asphalt-montmorillonite (MMT) composite, silylation-modification characteristics of cation ($Na^+$) exchanged K-10 (Na-MMT-K) using 3-aminopropyltriethoxysilane (APS) were studied and the optimal conditions of its silylation-modification process were proposed by use of the results of instrumental analysis, including FTIR, XRD, NMR and TGA, on silylation-modified Na-MMT-K (S-Na-MMT-K) under various conditions. According to FTIR analysis on S-Na-MMT-K, its peak-strengths of Si-O, -$NH_2$, -$CH_2$- and -OH, correlated with APS silylation-modification reaction, were compared each other. As a result, its optimal conditions including APS-MMT reacting period, APS-stirring period prior to APS-MMT reaction, APS concentration and reaction temperature were turned out to be 2~3 h, 20 min, 7.5 w/v% and $50^{\circ}C$, respectively. In addition, the optimal conditions induced from the results of TGA were also nearly consistent to those according to the results of FTIR analyses. These optimal conditions were turned out to be almost consistent to those drawn according to a criterion from XRD results suggested previously by Lee et al., by which the criterion was validated.

The Elderly Health and Dietary Management in Gyeonggi Province II - Comparison with Younger Old and Older Old - (경기지역 노인의 건강과 식생활관리 II - 75세 미만의 젊은 노인과 75세 이상 고령 노인 비교 -)

  • Rhie Seung-Gyo;Choi Mi-Yong;Won Hyang-Rye
    • The Korean Journal of Community Living Science
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    • v.17 no.1
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    • pp.141-154
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    • 2006
  • The purpose of this study is to provide the information of the aged olds for which basic data are almost no available. The subjects were divided on the base of age 75. The elderly under 75 were named 'the young olds' and over 75 were 'the aged olds'. The aim of this research is to promote health and to improve nutrition, and the survey was made for health promotion behaviors, habits against health risk, dietary management status and diet intake. And it was conducted by 24 hr-recall method and analyzed by nutrients intake. 242 subjects were collected in 12 cities or counties in Gyeonggi Province and 20 elderly people (10 male and 10 female) were selected out of 1 village in each district. Questionnaire about health behavior and dietary management was carried out by interview method through regional home extension workers. Statistical analyses were made by SAS (version 8.1) and Chi-square tests and General Linear Models were used. Out of the subjects the aged olds over 75 was 31.9%, elementary school educated (93.5%), with spouse (40.3%), with adult children(28.6%), monthly living cost of 500-1,000 thousand won(40.3%). Mean age was 78.82 years compared with 69.75 years of the young olds. 46.8% of the aged olds used monthly pocket money over 1000 won and it was lower than 63.3% of the young olds. Only half of the aged olds had regular exercise of walking (77.8%) or with athletic equipment (17.8%). However, the young olds did more frequent walking (82.1 %) and less exercise with athletic equipment (4.8 %), which was significantly different. Kinds of disease were different with the young or the aged olds, as more proportion of cardiovascular disease(37.9%) for the young olds and joint lumbago neuralgia(41.6%) for the aged olds. Dietary management was good (3 meals per day: 93.4%, fixed mealtime: 72.4%, and regular amount: 79.9%). But there was significant difference in side dish varieties and kinds of snacks; for the aged olds only 8% had over 5 sorts (compared with 18.8% of the young olds) and the kinds of snacks were cookie, candy, juice, carbonated beverage for the aged olds (compared with noodle, milk, soybean-milk for young olds). The ratio of nutrients intake (energy, riboflavin and niacin) with RDA was significantly higher for the aged olds than that of the young olds. The surveyed subjects had no difficulties in Activities of Daily Living (ADL), but some of the aged olds had difficulties in Instrumental Activities of Daily Living (IADL) like housekeeping, using transportation, going shopping and making phone calls. These results suggest that low quality of life is linked with low economic status of the rural elderly and congregate meal at village hall would be required because of the lack of side dishes variety for the aged olds. And nutrition education program about good snacks and exercise practice would be needed for the aged olds. By operating nutrition education program the aged olds would enjoy better quality life maintaining or ameliorating IADL abilities.

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The Elderly Health and Dietary Management in Gyeonggi Province - Comparison with Gender Difference - (경기지역 노인의 건강과 식생활관리 I - 노인의 성별 비교 -)

  • Won Hyang-Rye;Rhie Seung-Gyo;Choi Mi-Yong
    • The Korean Journal of Community Living Science
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    • v.17 no.1
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    • pp.123-139
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    • 2006
  • The purpose of this study is to search how to promote health and improve nutrition and health care of the elderly people in rural area. Behaviors for health promotion and habits against health risk were surveyed. Dietary management was analyzed for surveyed nutrient intake by 24 hr -recall method. 242 subjects were collected in 12 cities or counties in Gyeonggi Province and 20 elderly people (10 male and 10 female) were selected out of 1 village in each district. Questionnaire for health behavior and dietary management was carried out by trained interviewers. Statistical analyses were made by SAS (version 8.1) and Chi-square tests and General Linear Models were used. Characteristics of the elderly people were 61-74 year-olds (68.2%), elementary school educated (78.4%), with spouse (51.7%), monthly living cost of 500-1,000 thousand won(43.4%), and monthly pocket money of 50-100 or 100-200 thousand won(33.5%, 26.5%). 41.4% of the subjects checked up medical examination regularly. The alcohol drinking status was significantly different according to gender: high no-drink rate of female (52.5%) and low no-drink rate of male (25.6%). Kinds of disease were different according to gender: higher proportion of cardiovascular disease(46.3%) and diabetes mellitus(8.1 %) in male and joint lumbago neuralgia(44.4%) and osteoporosis(8.6%) in female. Gastrointestinal complaints were nausea (69.0%) and chronic indigestion (17.8%). Constipation (12.0%) and vomiting (4.3%) were more frequent in female. Dietary management was good (3 meals per day: 93.4%., dining with family: 72.4%, regular mealtime: 72.4%, and 3-4 times of snacks per week: 44.9%) except side dish taking of 3-4 kinds only. However, almost one-third of the female elderly ate alone (30.6%) which was well compared with one-fifth of the male (19.7%). And food and nutrients intake were not significantly different according to gender except that male elderly's intake of energy and protein was lower than that of female's. The surveyed subjects had no difficulties in Activities of Daily Living (ADL), but some female elderly had some difficulties with Instrumental Activities of Daily Living (IADL) like working at home, using transport, and going shopping. These results suggest that low quality of life linked with low economic status of the rural elderly and that congregate meal at village hall would be required for the female elderly eating alone. For the undernourished male elderly, it would be needed to provide snacks and to establish nutrition and health surveillance system.

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Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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