• Proceedings of the PSK Conference
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• 2003.04a
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• pp.284.3-285
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• 2003

Talniflumate is a potent analgesic and anti-inflammatory drug widely prescribed in rheumatoid diseases. The purpose of this work was to develop and validate a specific and robust method for the simultaneous determination of talniflumate and its metabolite, niflumic acid, in human plasma. Indomethacin was used as an internal standard (IS). (omitted)

• Bulletin of Food Technology
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• v.22 no.1
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• pp.21-28
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• 2009

• Proceedings of the PSK Conference
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• 2000.04a
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• pp.217.2-217.2
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• 2000

• Proceedings of the PSK Conference
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• 2002.04a
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• pp.223.2-223.2
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• 2002

• Proceedings of the PSK Conference
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• 2001.10a
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• pp.305.1-305.1
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• 2001

• 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.

• Journal of fish pathology
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• v.20 no.2
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• pp.139-145
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• 2007

To decrease stress in eel (Anguilla japonica) during its culture or transportation, aspirin (ASA) known as analgesic, antiinflammatory and antithrombic agent was administrated by dipping or oral routes. Concentrations of aspirin (ASA) and salicylic acid (SA) in eel plasma were simultaneously measured by a high performance liquid chromatography (HPLC). The plasma was acidified with 0.2 M HCl and 0.2 M orthophosphoric acid, and mixed with acetonitrile. ASA and SA extracted with acetonitrile were analyzed by the HPLC equipped with reversed phase Novapak C18 column (4 ㎛ silica, 150×4 mm) and UV detector(237 nm). The mobile phase consisted of 740 ㎖ water, 900 ㎕ orthophosphoric acid (85%) and 180 ㎖ acetonitrile. The retention times of ASA, SA and 2-methylbenzoic acid(MBA) were 4.8 min, 8.4 min and 11.5 min, respectively. The limit of quantification was 0.01 ㎍/㎖ for SA and 0.05 ㎍/㎖ for ASA. The mean recovery from eel plasma was 70.8～99.6% for ASA and 95.2～100.3% for SA. This HPLC method was applied to analyze ASA and SA of eel plasma after either dipping in a concentration of 20 ppm or feeding the feed supplemented with 50 ㎎/kg BW. Only SA was detected in eel plasma after the administration of ASA by dipping or oral routes because the drug was quickly decomposed into SA in eel plasma. The amount of SA in eel plasma reached the highest value at 3hr in dipping and 7 days in oral administration. When the ASA-administrated eel were kept in ASA free aquaria, 0.02-0.03 ㎍/㎖ of SA were detected 48 hr after the administration in both routes.

• Journal of Nutrition and Health
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• v.31 no.8
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• pp.1315-1323
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• 1998

Effect of oral taurine supplementation on plasma total and phospholidpid -fatty acid profiles and their metabolism were evaluated in healthy female adults. Among twenty five female volunteers(23.6$\pm$0.3 years old ) participated in the taruine supplementation program(6g taurine /day), twenty four subjects succesfully completed the 2 week program , and only nine subjects continued to take taurine for another 2 weeks. Levels of plasma fatty acids and taruine were measured by gas-liquid chromatobraphy and an automated amino acid analyzer based on ion exchange chromatography, respectively. Plasma taurine concentration s of the subjects were 108. 7$\pm$3.4 , 184.2$\pm$8.2 and 235.9$\pm$77.0$\mu$emol/L at 0 , 2 and 4 weeks of taurine supplementation. Fatty acid compositions and elongation and desaturation indices of polyunsaturated fatty acids (PUFA) in plasma total lipids were not influenced by oral taurine supplementation. However, fatty acid compositions and their metabolism in plasma phospholipids were significantly affected by taurine supplementation in female adults. Compared to the values for 0 week, the percentage of saturated fatty acids (SFA) in plasma phospholipid was significantly lowered at 2 weeks, but elevated at 4 weeks of taurine supplementation. In contrast , the percentage of phospholipid PUFA significantly increased at 2 weeks and decreased at 4 weeks of taurine supplementation from to the values for 0 weeks. Foru weeks of oral taurine supplementation signifinatly elevated the eongation index(20 : 4$\omega$6 ⇒22 : 4 $\omega$6, p<0.01), and decreased the desaturation index (20 : 3 $\omega$6 ⇒20 : 4 $\omega$6 , p<0.01) of $\omega$6 fatty acids in plasma phospholipids. Plasma taurine concentration was positively correlated with the percentage of 14 : 0 fatty acids and the enlongation index o f$\omega$3 fatty acids(20 : 5 $\omega$3 ⇒22 : 5 $\omega$3), and thenegatively correlated with the percentage of 20 : 0 in plasma phospholipids. These results indicate that oral taurine supplementation for 4 weeks signidicantly elelvated the percentage of SFA, and lowered the percentage of PUFA in plasma phospholipids with no influence on plasm total fatty aicd composition in healthy female adults.

• Journal of Pharmaceutical Investigation
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• v.12 no.2
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• pp.45-53
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• 1982

The effects of mixture of tween 20 and span 20 or span 80 on griseofulvin absorption in rabbit were studied. The plasma concentration of griseofulvin in blood samples was determined by high pressure liquid chromatographic procedure. Griseofulvin suspension with 0.05% surfactant increased mostly drug absorption and produced about two times higher plasma level of griseofulvin than that of the suspension with 1% and 0.1% surfactant. Surfactants with H.L.B. value 4.3 resulted $2.74{\mu}g/ml$ of maximum plasma levels of griseofulvin at 18 hours after its oral administration and surfactants with H.L.B. value 16.7 resulted $0.56{\mu}g/ml$ of peak plasma levels of griseofulvin at 1 hour after its oral administration.

• Archives of Pharmacal Research
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• v.17 no.6
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• pp.458-461
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• 1994

A new high-performance liquid chromatographic method with column switching has been onto a Bondapak phenyl/corsil $(37-50{\;}{\mu}m)$ precolumn and polar plasma components were washed with 0.06 M borate burffer. After valve switching, the concentrated drug were eluted in the back-flush mode and separated on a ${\mu}-Bondapak$ C18 column with acetonitrilke-phosphate buffer as the mobile phae. The method showed excellent precision, accuracy and speed with detection limit of $0.01{\;}{\mug}/ml^{-1}$. Total analysis time per smaple was less than 20 min and the coefficients of variation for intra and inter-assay were less than 5.635. This method has been successfully applied to plasma smaples from eats after oral administration of omeprazole.